تفاعل #319906

معادلة التفاعل

title compound

3,3a, 4,5-tetrahydro-3a-methoxycarbonyl-N-[4'-(trifluoromethyl)phenyl]-2H-benz[g]indazole-2-carboxamide

triethylamine

ethyl (chlorosulfenyl) (1-methylethyl)carbamate

Ethyl (chlorosulfenyl)(1-methylethyl)carbamate

→

title compound

المردود 85.7%

3,3a, 4,5-Tetrahydro-3a-methoxycarbonyl-N-[4-(trifluoromethyl)phenyl]-N-[N'-(1-methylethyl)-N'-(ethoxycarbonyl)aminosulfenyl]-2H-benz[g]indazole-2-carboxamide

المردود 85.7%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىThe crude mixture was purified by silica column chromatography

الإجراء التجريبي

To a solution of the title compound of Step B (2.0 g, 4.8 mmol) in 50 ml methylene chloride cooled to 0° C. was added triethylamine (1.0 g, 0.01 mol) and ethyl (chlorosulfenyl) (1-methylethyl)carbamate from Step D (1.4 g, 7.7 mmol). The mixture was allowed to warm to room temperature and stirred for one hour. The crude mixture was purified by silica column chromatography using ether-hexane (1:2) as eluent. The title compound (2.38 g) was obtained in about 90% purity (mp: 130°-134°). Extraction of the product with ether-hexane (2:1) gave 1.8 g of highly pure material mp: 139°-140° C.

المصدر