反応 #58348

反応方程式

(±)-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

収率 91.6%

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

収率 91.6%

溶媒

dichloromethane

dichloromethane

pyridine

反応条件

後処理

1. 1
   抽出the reaction mixture is extracted with 6 N sodium hydroxide solution, 2 N hydrochloric acid and finally water
2. 2
   その他The organic phase is dried
3. 3
   濃縮concentrated

実験手順

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.

出典