Category: 513-74-6

Adding a certain compound to certain chemical reactions, such as: 513-74-6, name is Ammonium carbamodithioate, belongs to amides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 513-74-6, Safety of Ammonium carbamodithioate

Step 89.2: Ammonium dithiocarbamate (208 mg, 1.89 mmol) and 72 (X = Br) (200 mg, 0.63 mmol) in anhydrous MeOH (10 mL) was stirred for 10 mins. The resulting cream precipitate was collected by filtration, resuspended in acetic acid (10 mL) and refluxed for 1 hr. The reaction was cooled to room temperature and diluted with ice cold water. The resulting green precipitate was collected by filtration, redissolved in (CH2CI2:Me0H 95:5, 100 mL) and dried (Na2SO4). The pale green solution was concentrated in vacuo to give 4-(5-bromopyrazolo[1 ,5-a]pyridin-3-yl)thiazole-2(3/-/)-thione (73: X = Br) (136 mg, 70 percent) that is stored in the freezer. 1H NMR delta (400 MHz, d6-DMSO) 13.59 (br s, 1 H), 8.74 (d, J 7.3 Hz, 1H1), 8.51 ( s, 1 H ), 8.22 (d, J 1.8 Hz, 1H), 7.27 (s, 1 H1), 7.19 (dd, J 7.3, 2.1 Hz, 1 H). LCMS (APCI+) 312 (MH+ with 79Br, 100percent), 314 (MH+ with 81Br, 100percent).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ammonium carbamodithioate, and friends who are interested can also refer to it.

Reference:
Patent; AUCKLAND UNISERVICES LIMITED; WO2009/8748; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 513-74-6, name is Ammonium carbamodithioate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: amides-buliding-blocks

Methyl Dithiocarbamate (I) [2] In a 500mL three-necked flask, provided with a gas-inlet tube, a stirrer, and a gas outlet combined with a thermometer, are placed dry THF(140mL) and carbon disulfide (16.7g, 0.22mol). Ammonia is then introduced with continuous stirring, the flow of ammonia being adjusted in such a way that a slow stream is leaving the flask. The temperature is allowed to rise to 40-45 °C and is kept at that level by occasional cooling. When, after 1h, no more heat is evolved and the temperature has dropped to 35 °C, the flask is evacuated (rotary evaporator) to remove some dissolved ammonia. Water (25mL) is then added to dissolved the white precipitate. To the resultant mixture of THF and aqueous ammonium dithiocarbamate, dimethylsulfate (25.2g, 0.2mol) is added with vigorous stirring. During the addition (which requires 30min), the temperature of the mixture is allowed to rise to 45-50 °C and is maintained at that level for 15 min by occasional cooling. Then, concentrated aqucous ammonia (5mL) is added to destroy excess dimethyl sulfate and stirring is continued for 15min. The upper layer is separated and dried with magnesium sulfate (without being washed). The aqueous layer is extracted with EA (3*20mL) and the organic phases are combined. The solution is concentrated in a water-pump vacuum and the last traces of solvent are removed at 0.5-1 torr by means of an oil pump to leave nearly pure methyl dithiocarbamate(I); yield: 20g (93percent, calculated on dimethyl sulfate).

The synthetic route of 513-74-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shin Nippon Biomedical Laboratories, Ltd.; SUZUKI, Nobuyuki; YAMASHITA, Hidetoshi; (156 pag.)EP3018125; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 513-74-6, name is Ammonium carbamodithioate, belongs to amides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 513-74-6, HPLC of Formula: CH6N2S2

Step 89.2: Ammonium dithiocarbamate (208 mg, 1.89 mmol) and 72 (X = Br) (200 mg, 0.63 mmol) in anhydrous MeOH (10 mL) was stirred for 10 mins. The resulting cream precipitate was collected by filtration, resuspended in acetic acid (10 mL) and refluxed for 1 hr. The reaction was cooled to room temperature and diluted with ice cold water. The resulting green precipitate was collected by filtration, redissolved in (CH2CI2:Me0H 95:5, 100 mL) and dried (Na2SO4). The pale green solution was concentrated in vacuo to give 4-(5-bromopyrazolo[1 ,5-a]pyridin-3-yl)thiazole-2(3/-/)-thione (73: X = Br) (136 mg, 70 percent) that is stored in the freezer. 1H NMR delta (400 MHz, d6-DMSO) 13.59 (br s, 1 H), 8.74 (d, J 7.3 Hz, 1H1), 8.51 ( s, 1 H ), 8.22 (d, J 1.8 Hz, 1H), 7.27 (s, 1 H1), 7.19 (dd, J 7.3, 2.1 Hz, 1 H). LCMS (APCI+) 312 (MH+ with 79Br, 100percent), 314 (MH+ with 81Br, 100percent).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ammonium carbamodithioate, and friends who are interested can also refer to it.

Reference:
Patent; AUCKLAND UNISERVICES LIMITED; WO2009/8748; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 513-74-6, These common heterocyclic compound, 513-74-6, name is Ammonium carbamodithioate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: Following literature procedures,1 ammonia gas was bubbled into carbon disulfide 1 (16.7g, 0.22 mol) in THF (100 ml) keeping the temperature below 45 ¡ãC. After 1 hr, the reaction was stopped by allowing the temperature to decrease to rt. The excess ammonia gas was removed by streaming N2 for 30 min or by rotary evaporation under vacuum. The precipitate was collected by filtration to afford white solid ammonium dithiocarbamate 2 (23.1 g, 96percent). Methyl iodide (17.8 g, 0.125 mol) was added to a solution of 2 (5.5 g, 0.05 mol) in acetone (100 ml) at rt and the mixture was stirred for 24 hr. The solid was collected by filtration, washed with chilled acetone (20 ml) and dried under vacuum to provide white solid S,S?-dimethyliminodithiocarbonate hydroiodide ammonium iodide 3 (18.9 g, 96percent). 3 (7.9 g, 0.02 mol) was treated with sat. aq. NaHCO3 solution (100 ml x 2) and the organic products extracted with dichloromethane (50 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo to a clear, colorless liquid 4 (2.3 g, 95percent). 1H NMR (400 MHz, CDCl3) delta 8.88 (s, 1H), 2.42 (s, 6H). 13C NMR (101 MHz, CDCl3) delta 172.10, 14.50. HRMS (ESI+) m/z calcd for C3H8N+ 122.0098, found 122.0096.

Statistics shows that Ammonium carbamodithioate is playing an increasingly important role. we look forward to future research findings about 513-74-6.

Reference:
Article; Pollock, Julie A.; Kim, Sung Hoon; Katzenellenbogen, John A.; Tetrahedron Letters; vol. 56; 44; (2015); p. 6097 – 6099;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 513-74-6,Some common heterocyclic compound, 513-74-6, name is Ammonium carbamodithioate, molecular formula is CH6N2S2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

0.69g Ammonium dithiocarbamate were dissolved in 10ml MeOH and 1.47g 4-(2- bromoacetyl)-1-methylpyridinium bromide were added. After 2h at ambient temperature the mixture was refluxed. After cooling the precipitate was filtered, washed with MeOH and dried. Yield: 0.15g 1H-NMR (DMSO-d6) delta 4.32(s, 3H), 8.32(s, 1 H), 8.45(d,2H; J=6.9Hz), 9.08(d,2H; J=6.8Hz), 14.1 (br s, 1 H) 13C-NMR (DMSO-c/6) delta 47.3, 121.6, 122.5, 136.6, 141.3, 145.9, 190.2

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ammonium carbamodithioate, its application will become more common.

Reference:
Patent; SANDOZ AG; KREMMINGER, Peter; STURM, Hubert; WO2013/34718; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics