Category: 112101-81-2

112101-81-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The oily mass of formula-IIId obtained in step (i) (c) is taken and dissolved in 125.0ml of n-butanol. The solution is heated to 100C under nitrogen atmosphere. A solution of 29.1gms (0.1mole) of 2-(2-ethoxyphenoxy) ethyl iodide in 30ml of n-butanol is slowly added at 100-105C over a period of 3-4 hrs and maintained at 100-110C for further 4hrs. Then n-butanol is distilled off under vacuum at temp not exceeding 80C. The resulting mass is cooled to 20C and vacuum released under nitrogen atmosphere. 50.0ml of n-hexane is added to the mixture. An uniform slurry is made and the product is allowed to solidify at 0-5C. It is filtered and washed with 50ml of n-hexane. The product is dried at 40-50C under vacuum to obtain 22.0gms solid of quarternary ammonium salt of formula-IId. Recrystallized (from acetonitrile) has the following characteristics. MR : 200-208C 1H NMR : (200MHz, DMSO-d6) delta 1.15-1.19 (d, 3H), 1.28-1.31 (t, 3H), 2.60-2.70 (m, 2H), 3.40 (broad, 2H), 3.46-3.54 (m, 3H), 3.9 (s, 3H), 3.87-4.01 (dd, 4H), 4.20- 4.22 (t, 2H), 6.92-7.67 (aromatic, 11H), 8.15 (s, imine, 1H) IR : (KBr), 3305, 3210, 2930, 1632, 1609, 1494, 1439, 1330, 1282, 1252, 1456, 1075, 1011, 533, 522, 454 cm-1

The synthetic route of 112101-81-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NATCO PHARMA LIMITED; WO2004/16582; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

112101-81-2, A common compound: 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, belongs to amides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

EXAMPLE 3;Preparation of Tamsulosin HydrochlorideTamsulosin Hydrochloride is also prepared according to this example by first repeating the initial reaction, cooling, and filtering steps of Example 2 to produce the filtrate at 0 C.Instead of using ammonia, the filtrate is then alkalinized with DIEA until a pH of 8.5 is obtained, and the desired product is extracted with 2 x 50 mL of AcOEt. The combined organic layers are then extracted twice with 50 mL of water at pH 6 (adjusted with HCl). The EPO aqueous phases are combined and the pH is again adjusted to 8.5 with DDEA, and the product is then extracted with 2 x 25 mL of AcOEt.The combined organic phases obtained from the extractions are dried over Na2SO4 and the solvent is evaporated to obtain 3.28 g of crude tamsulosin. The content of byproduct as determined by HPLC method 1 was 0.261% (area percentage).The residue is dissolved in ethanol (32 mL) and 1.65 mL (7.76 mmol) of ethanol HCl 4.7 N are charged. Then, the mixture is cooled down to 0 C and the solid is collected by filtration, washed with ethanol and dried in vacuum at 60 C until constant weight to yield 2.17 g (4.87 mmols, 26% molar yield) of tamsulosin hydrochloride. By subsequent analysis, the content of by-product (formula (VE)) by HPLC method 1 at this stage is 0.08 area %.The tamsulosin hydrochloride thus obtained is further purified by repeating twice the following procedure: treating with 29 mL of ethanol at 78 C, stirring for 30 minutes, cooling to 0 C, filtering, washing with ethanol and then drying at 60 C in vacuum until constant weight. After drying, 1.98 g of tamsulosin hydrochloride are obtained (4.45 mmols, 91% partial molar yield). (Assay: 100.21%; IR: matches the standard; melting point: 227.4-229.3 C; chemical purity: 99.31 area % by HPLC method 1; XRD (20), see Figure 1; content of byproduct (formula (VII)) by HPLC method 1 : 0.02 area %)

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDICHEM, S.A.; WO2007/4077; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

The chemical industry reduces the impact on the environment during synthesis 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, I believe this compound will play a more active role in future production and life. 112101-81-2

10 g of (-)- (R)-5- (2- (2- (2-ethoxyphenoxy) ethylamino)-1-propyl)-2-methoxybenzene sulphonamide hydrochloride (TH) from Example 2 is recrystallised from mixtures of methanol and ethanol. Analysis : Methanol HPLC-composition Quantity of Yield HPLC-composition to ethanol of the starting raw solvent of the product* ratio material* used 100 : 0 TH 86. 1 % 120 mi 7. 77 g TH 95. 84 % impurity (2) 1. 53 % (77. 7 %) impurity (2) 0. 09 % impurity (3) 2. 84 % impurity (3) 0. 0 % impurity (4) 1. 79 % impurity (4) 0. 24 % impurity (5) 0. 98 % impurity (5) 0. 05 % impurity (6) 6. 17 % impurity (6) 3. 73 % 90 : 10 TH 86. 1 % 75 g TH 95. 5% impurity (2) 1. 53 % (77, 5%) impurity (2) 0. 12 % impurity (3) 2. 84 % impurity (3) 0. 0 % impurity (4) 1. 79 % impurity (4) 0. 31 % impurity (5) 0. 98 % impurity (5) 0. 08 % impurity (6) 6. 17 % impurity (6) 3. 94 % 70 : 30 TH 86. 1 % 210 ml 7, 78g TH 95. 9 % impurity (2) 1. 53 % (77. 8 %) impurity (2) 0. 12 % impurity (3) 2. 84 % impurity (3) 0. 0 % impurity (4) 0. impurity 0. 31 % impurity (5) 1. 79 % impurity (5) 0. 08 % impurity (6) 6. 17 % impurity (6) 3. 49 % 50 : 50 TH 86. 1 % 340 ml 7. 41 g TH 99. 27% impurity (2) 1. 53 % (74. 1 %) impurity (2) 0. 15 % impurity (3) 2. 84 % impurity (3) 0. 0 % impurity (4) 0. 98 % impurity (4) 0. 32 % impurity 1. 79 % impurity (5) 0. 08 % impurity (6) 6. 17 % impurity (6) 0. 0 % 30 : 70 TH 86. 1 % 500 ml 7. 55 g TH 99. 28 % impurity (2) 1. 53 % (75. 5 %) impurity (2) 0. 17 % impurity (3) 1. 79 % impurity (3) 0. 0 % impurity (4) 0. 98 % impurity (4) 0. 32 % impurity (5) 1. 79 % impurity (5) 0. 10 % impurity (6) 6. 17 % impurity (6) 0. 0 % * impurity (2) = 5-((R)-2-amino-1-propyl)-2-methoxybenzenesulphonamide impurity (3) = 2-(2-ethoxyphenoxy) ethylbromide impurity (4) = N-(2-(2-ethoxyphenoxy) ethyl)-5-(2-(2-(2-ethoxyphenoxy) ethyl) amino)-1-propyl)-2-methoxybenzenesulphonamide impurity (5) = 5-(2-(bis-(2-(2-ethoxyphenoxy) ethyl) amino)-1-propyl)-2-methoxybenzenesulphonamide impurity (6) = 1,2-bis (2-ethoxyphenoxy) ethane (6)

The chemical industry reduces the impact on the environment during synthesis 112101-81-2. I believe this compound will play a more active role in future production and life.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; WO2005/63702; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

112101-81-2, A common compound: 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, belongs to amides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

7.0 g of recrystallised (-)-(R)-5-(2-(2-(2-ethoxyphenoxy) ethylamino)-1-propyl)-2- methoxybenzenesulphonamide hydrochloride (TH) from Example 3 is recrystallised from mixtures of methanol and ethanol. Analysis : Methanol to HPLC-composition of Quantity Yield HPLC-composition of ethanol the starting raw of solvent the product* ratio material* used 100 : 0 TH 95. 84 % 90 ml 5. 44 g TH 97. 77 % impurity (2) 0. 09 % (77. 7%) impurity (2) 0. 0 % impurity (3) 0. 0 % impurity (3) 0. 0 % impurity (4) 0. 24 % impurity (4) 0. 04 % impurity (5) 0. 05 % impurity (5) 0. 0 % impurity (6) 3. 73 % impurity (_) 2. 19 % 90 : 10 TH 95. 5 % 110 ml 5. 64 g TH 97. 53 % impurity (2) 0. 12 % (80. 6%) impurity (2) 0. 12 % impurity (3) 0. 0 % impurity (3) 0. 0 % impurity (4) 0. 31 % impurity (4) 0. 06 % impurity (2 0. 08 % impurity (5) 0. 00 % impurity (6) 3. 94 % impurity (6) 2. 41 % 70 : 30 TH 95. 9 % 160 ml 5. 70 g TH 99. 89 % impurity (2) 0. 12 % (81. 4%) impurity (2) 0. 0 % impurity (3) 0. 0 % impurity (3) 0. 0 % impurity 0. 31 % impurity (4) 0. 05 % impurity (5) 0. 08 % impurity (5) 0. 0 % impurity (6) 3. 49 % impurity (6) 0. 0 % 50 : 50 TH 99. 27 % 230 ml 5. 95g TH 99. 85 % impurity (2) 0. 15 % (85. 0%) impurity (2) 0. 0 % impurity (3) 0. 0 % impurity (3) 0. 0 % impurity (4) 0. 32 % impurity (4) 0. 06 % impurity (5) 0. 08 % impurity (5) 0. 0 % impurity (6) 0. 0% impurity 0. 0% 30 : 70 TH 99. 28 % 340ml 5. 98 g TH 99. 81 % impurity (2) 0. 17 % (85. 4%) impurity (2) 0. 02 % impurity (3) 0. 0 % impurity (3) 0. 0 % impurity (4) 0. 32 % impurity (4) 0. 08 % impurity (5) 0. 10 % impurity (5) 0. 0 % impurity (6) 0. 0 % impurity (6) 0. 0 % * impurity (2) = 5-((R)-2-amino-1-propyl)-2-methoxybenzenesulphonamide impurity (3) = 2-(2-ethoxyphenoxy) ethylbromide impurity N- (2- (2-ethoxyphenoxy) ethyl)-5- (2- (2- (2-ethoxyphenoxy) ethyl) amino)-1-propyl)-2-methoxybenzenesulphonamide impurity (5) = 5-(2-(bis-(2-(2-ethoxyphenoxy) ethyl) amino)-1-propyl)-2-methoxybenzenesulphonamide impurity (6) = 1,2-bis (2-ethoxyphenoxy) ethane (6)

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; WO2005/63702; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics