반응 #565338

반응 방정식

2-amino-1-butanol

N,N′-dicyclohexylcarbodiimide

1-bromocyclopropanecarboxylic acid

N-hydroxysuccinimide

→

1-bromo-N-[(1-hydroxymethyl)propyl]-cyclopropane-1-carboxamide

수율 76.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGit is stirred for 2 hours at room temperature
2. 2
   여과After dilution with methylene chloride, it is filtered
3. 3
   농축concentrated by evaporation
4. 4
   기타the residue is chromatographed on silica gel with ethyl acetate/hexane

실험 절차

7.45 g of N,N′-dicyclohexylcarbodiimide is added at 0° C. under nitrogen to a solution of 5.0 g of 1-bromocyclopropanecarboxylic acid 4 and 4.18 g of N-hydroxysuccinimide in 87 ml of methylene chloride, and it is stirred for 1.5 more hours. Then, 7.46 ml of 2-amino-1-butanol is added, and it is stirred for 2 hours at room temperature. After dilution with methylene chloride, it is filtered, concentrated by evaporation, and the residue is chromatographed on silica gel with ethyl acetate/hexane. 5.44 g of 1-bromo-N-[(1-hydroxymethyl)propyl]-cyclopropane-1-carboxamide 78 is obtained as a yellowish oil.

출처