HRID247560

反应详情

EQUATION

反应方程式

HRID 247560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At -70° C., 73 ml of a 1.7-molar butyllitium solution in hexane is added dropwise to a solution of 18.6 g of the dimethyl ester of methanephosphonic acid in 280 ml of tetrahydrofuran; the mixture is stirred for 15 minutes and a solution of 10.5 g of 2-methylhept-5-ynoic acid ethyl ester in 48 ml of tetrahydrofuran is gradually added thereto. The mixture is stirred for 4 hours at -70° C., neutralized with acetic acid, and evaporated under vacuum. The distillation of the residue under vacuum at 0.6 torr and 130° C. yields 10.8 g of the title compound as a colorless fluid.

WORKUP

后处理

  1. stirringThe mixture is stirred for 4 hours at -70° C.
  2. customevaporated under vacuum
  3. distillationThe distillation of the residue under vacuum at 0.6 torr and 130° C.