HRID632564

反应详情

EQUATION

反应方程式

HRID 632564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2,4-bis-benzyloxy-5-isopropenyl-N,N-di-prop-2-ynyl-benzamide (0.545 g, 1.21 mmol) in ethyl acetate (10 mL) was added 4-pentyn-1-ol (0.30 mL, 3.2 mmol) and RhCl(PPh3)3(0.161 g, 0.17 mmol). Solvent was removed under vacuum, and the mixture stirred at room temperature overnight. Additional 4-pentyn-1-ol (2.5 mL, 26 mmol) and RhCl(PPh3)3 (0.155 g, 0.17 mmol) were added and the mixture stirred for 48 hours. The mixture was loaded onto a silica gel column and eluted with 7:3 ethyl acetate:heptane to yield the desired product (0.254 g, 39% yield). LC/MS: m/z 534.25 [M+H]+

WORKUP

后处理

  1. customSolvent was removed under vacuum
  2. stirringthe mixture stirred for 48 hours
  3. washeluted with 7:3 ethyl acetate