تفاعل #319911

معادلة التفاعل

title compound

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

triethylamine

hexyl (chlorosulfenyl)(methyl)carbamate

→

title compound

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

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرى(prepared in a manner similar to Example 1, Step D), (2.5 g 75% pure) dropwise at 0° C
2. 2
   تركيزThe reaction mixture was concentrated under high vacuum

الإجراء التجريبي

To a suspension of the title compound of Step E above (2.2 g, 0.005 mol) in 25 ml methylene chloride cooled to 0° C. was added triethylamine (1.0 g) and hexyl (chlorosulfenyl)(methyl)carbamate, (prepared in a manner similar to Example 1, Step D), (2.5 g 75% pure) dropwise at 0° C. The mixture was stirred at room temperature for additional one hour. The reaction mixture was concentrated under high vacuum and subjected to silica gel column chromatography using hexane-ether (1:1) as an eluent. The title compound (2.5 g) was obtained, melting point 128°-129° C. in high purity.

المصدر