ChemicalBook CAS DataBase List CarbaMic acid, N-(4-broMo-2-nitrophenyl)-, 1,1-diMethylethyl ester

CarbaMic acid, N-(4-broMo-2-nitrophenyl)-, 1,1-diMethylethyl ester synthesis

6synthesis methods

Product Name:CarbaMic acid, N-(4-broMo-2-nitrophenyl)-, 1,1-diMethylethyl ester
CAS Number:327046-79-7
Molecular formula:C11H13BrN2O4
Molecular Weight:317.14

1228392-59-3 Synthesis

di-tert-butyl 4-bromo-2-nitrophenylcarbamate

1228392-59-3
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CarbaMic acid, N-(4-broMo-2-nitrophenyl)-, 1,1-diMethylethyl ester

327046-79-7
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Yield: 82.8%

Reaction Conditions:

with potassium carbonate in acetonitrile at 35; for 1.5 h;

Steps:

1.2 Tert-butyl (4-bromo-2-nitrophenyl)carbamate
Tert-butyl N-(4-bromo-2-nitro-phenyl)-N-tert-butoxycarbonyl-carbamate 1b (7.12 g, 17.1 mmol) and potassium carbonate (7.08 g, 51.2 mmol) were dissolved in 140 mL of acetonitrile, the solution was heated to 35 °C and reacted for 1.5 hours.
The reaction solution was filtered, the filtrate was concentrated under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent: A system) to obtain tert-butyl (4-bromo-2-nitrophenyl)carbamate 1c (4.49 g, bright yellow solid), yield: 82.8%.
MS m/z (ESI): 216.8 [M+1-100]

References:

Zhejiang Hisun Pharmaceutical Co., Ltd.;CHEN, Lei;GUAN, Dongliang;BAI, Hua;GOU, Jun;ZHAO, Weifeng;WANG, Zhongli;LING, Long;MA, Yutao EP3459952, 2019, A1 Location in patent:Paragraph 0068; 0070

24424-99-5 Synthesis