Category: 21440-97-1

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 21440-97-1 as follows. SDS of cas: 21440-97-1

Example 16 General Procedure for Examples 16 to 30; A mixture of the appropriate aryl bromide (2.0 mmol), alkylene (2.2 mmol), N,N-dicyclohexylmethylamine (470 muL, 2.2 mmol) and tri-tert-butylphosphine (24 mg, 0.12 mmol) in dioxane (5 mL) was purged with nitrogen. Tris(dibenzylideneacetone)dipalladium (0) (55 mg, 0.06 mmol) was added and the mixture again purged with nitrogen and then stirred at room temperature. The reaction was monitored by LC/MS. If necessary, more catalyst was added. The reaction was diluted with ethyl acetate and filtered through a small amount of silica gel. The silica gel was rinsed with ethyl acetate and then methanol. The filtrates were kept separate and each concentrated under reduced pressure. The residues from the filtrates were analyzed for product by use of LC/MS. The product was purified by the methods described.; Step 3: (2E)-3-(2-Oxo-1,2-dihydrospiro[3,1-benzoxazine-4,1′-cyclohexan]-6-yl)but-2-enamide6-Bromospiro[4H-3,1-benzoxazine-4,1′-cyclohexan]-2(1H)-one (592 mg, 2.0 mmol), prepared in the previous step, and (E)-but-2-enamide (187 mg, 2.2 mmol) were reacted according to the General Procedure described above. By LC/MS, the methanol filtrate contained the product. The methanol filtrate was concentrated under reduced pressure to remove the solvent. The residue was taken up in ethyl acetate. Upon standing some solid precipitated. The solid was collected by filtration and dried under reduced pressure. By nuclear magnetic resonance (NMR) analysis, the solid contained ethyl acetate. The solid was taken up in methanol-methylene chloride and concentrated under reduced pressure. It was then taken up in methylene chloride and again concentrated under reduced pressure. This process was repeated two additional times and then the solid was dried under reduced pressure to give the title compound (50 mg, 8%) as a white solid, mp 204-207 C. (dec), MS m/z 301, MS m/z 299.

According to the analysis of related databases, 21440-97-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; US2009/197878; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 21440-97-1, The chemical industry reduces the impact on the environment during synthesis 21440-97-1, name is 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, I believe this compound will play a more active role in future production and life.

With a thermometer,Add 40g compound 17, to the 1L three-neck bottle of the condenser28.7 g carbazole, 32.3 g K2CO3, 0.62 g 1,10-Phenanthroline,Then 450 ml of DMF was added.Replace the air in the reaction system with nitrogen,Add 0.45 g of CuBr under nitrogen protection.Heat to 120 C for 10 h,After the TLC was monitored, the starting material was completely reacted and the stirring was stopped and lowered to room temperature.The reaction system is added to 3 volumes of water,The product was precipitated by stirring and filtered.The filter cake was completely dissolved in 500 ml of dichloromethane (DCM) and washed 3 times with water.150ml each time. The organic phase is dried and concentrated.The crude product was passed through a silica gel column to give compound 18 as a white solid, 43.1 g, yield 80.6%.

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, 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Xi’an Ruilian New Materials Co., Ltd.; Sun Jun; Zhang Hongke; Liu Kaipeng; Yang Yan; Yang Dandan; Gao Renxiao; (34 pag.)CN108912138; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 21440-97-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 21440-97-1 as follows.

Example 6 Preparation of 6-bromo-4,4-dimethyl-benzoxazine-2-one Lithium Salt Similarly, 6-bromo-4,4-dimethyl-benzoxazine-2-one (2.55 g) was reacted with lithium tert-butoxide (10 mL of 1M solution in THF). After evaporation a brownish solid was obtained (3.35 g; quant. yield) that was soluble in dimethyl pyrimidone (DMPU) without heating. 1H NMR (DMSO-d6) did not show a peak corresponding to a N-H group.

According to the analysis of related databases, 21440-97-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; US2005/250766; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 21440-97-1, name is 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, 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 21440-97-1, Formula: C10H10BrNO2

6-bromo-4,4-dimethyl-lH-3,l-benzoxazin-2-one (250 mg, 0.976 mmol) was dissolved in dimethylformamide (5 mL) and potassium carbonate (0.204 g, 1.46 mmol) was added. The suspension was stirred for 10 min and then iodoethane (0.158 mL, 1.95 mmol) was added. The reaction mixture was heated to 60C and stirred for 4 h. The reaction mixture was poured into ice/water and then extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine (2×20 mL). dried and concentrated. The crude oil was purified by flash chromatography to give the desired compound (0.275 g, 99%) as a colorless oil. LCMS: 0.98 min; ES+ 284/286 (M+H+); XH NMR (CHLOROFORM-d, 400MHz): delta (ppm) 7.43 (d,lH), 7.28 (s, 1H), 6.86 (d, 1H), 3.98 (q, 2H), 1.67 (s, 6H), 1.32 (t, 3H)

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, 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; SYNGENTA PARTICIPATIONS AG; CUTLER, Sean, R.; LACHIA, Mathilde, Denise; WENDEBORN, Sebastian, Volker; GODFREY, Christopher, Richard Ayles; SABBADIN, Davide; (82 pag.)WO2018/17490; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 21440-97-1, name is 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, 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. Recommanded Product: 21440-97-1

EXAMPLE 8 6-(4-Chloro-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]-oxazin-2-one Prepared according to Procedure A from 6-bromo-4,4-dimethyl -1,4-dihydro-benzo[d][1,3]oxazin-2-one and 4- chlorophenyl boronic acid. White solid: mp 255-257 C.; 1H-NMR (DMSO-d6) delta10.3 (s, 1H), 7.7 (d, 2H, J=8.52 Hz), 7.55 (m, 2H), 7.5 (d, 2H, J=8.52 Hz), 6.96 (d, 1H, J=8.52 Hz), 1.7 (s, 6H); MS (ESI) m/z 288 ([M+H]+, 70%); Anal. Calc. For C16H14CINO2: C, 66.79, H, 4.90, N, 4.87. Found: C, 66.34, H, 4.76, N, 4.75

The synthetic route of 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth; Ligand Pharmaceuticals, Inc.; US6444668; (2002); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 21440-97-1, name is 6-Bromo-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one, 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 21440-97-1, SDS of cas: 21440-97-1

A solution of 61(500 mg, 1.95 mmol), benzyl mercaptan (0.34 mL, 2.92 mmol), i-Pr2NEt (1.03 mL, 5.90mmol), Pd2(dba)3 (90 mg, 0.098 mmol) and XantPhos (113mg, 0.195 mmol) in dioxane (10 mL) was degassed with N2 for 5 min.The mixture was then heated to 100 C for 5 h. The crude reaction mixture was dry-loaded onto silica gel and purified via ISCO flash column chromatography(eluting with 40% EtOAc in hexanes) to afford 62 (550 mg, 94%).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Lotesta, Stephen D.; Marcus, Andrew P.; Zheng, Yajun; Leftheris, Katerina; Noto, Paul B.; Meng, Shi; Kandpal, Geeta; Chen, Guozhou; Zhou, Jing; McKeever, Brian; Bukhtiyarov, Yuri; Zhao, Yi; Lala, Deepak S.; Singh, Suresh B.; McGeehan, Gerard M.; Bioorganic and Medicinal Chemistry; vol. 24; 6; (2016); p. 1384 – 1391;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics