반응 #58348

반응 방정식

(±)-3,4-bis-cyclopropylmethoxy-N-[(1RS,2RS,5RS)-2-(3,4-dimethoxyphenyl)-5-hydroxycyclohexyl]benzamide

compound D1

(±)-3,4-bis-cyclopropylmethoxy-N-[(1RS,2RS,5RS)-2-(3,4-dimethoxyphenyl)-5-hydroxycyclohexyl]benzamide

→

title compound

수율 91.6%

(±)-3,4-Bis-cyclopropylmethoxy-N-[(1RS,2RS)-2-(3,4-dimethoxyphenyl)-5-oxo-cyclohexyl]-benzamide

수율 91.6%

용매

dichloromethane

dichloromethane

pyridine

반응 조건

후처리

1. 1
   추출the reaction mixture is extracted with 6 N sodium hydroxide solution, 2 N hydrochloric acid and finally water
2. 2
   기타The organic phase is dried
3. 3
   농축concentrated

실험 절차

A solution of 8.0 g of (±)-3,4-bis-cyclopropylmethoxy-N-[(1RS,2RS,5RS)-2-(3,4-dimethoxyphenyl)-5-hydroxycyclohexyl]benzamide (compound D1) in 80 ml of dichloromethane is added dropwise to a suspension of 10 g of chromium (III) oxide in 160 ml of dichloromethane and 16 ml of pyridine. After stirring for 2 h at room temperature, the reaction mixture is extracted with 6 N sodium hydroxide solution, 2 N hydrochloric acid and finally water. The organic phase is dried using sodium sulfate and concentrated. 7.3 g of the title compound of m.p. 150-151.5° C. are obtained.

출처