HRID1639434

反应详情

EQUATION

反应方程式

HRID 1639434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.2 g of dicyclohexycarbodiimide were added to a solution of 9.5 g of the product of Step C, 30 ml of methylene chloride and 3 ml of pyridine and the reaction mixture was stirred for half and hour. 6.8 g of (S)α-cyano-3-phenoxy-benzyl alcohol were added thereto and the mixture was stirred for an hour and half and filtered. The filtrate was washed with N hydrochloric acid, then with water until neutral, dried, and evaporated to dryness. The 15.3 g of oil residue were chromatographed over silica gel and eluted with a 97-3 mixture of benzene-ethyl acetate to obtain 12 g of (S)α-cyano-3-phenoxy-benzyl (1R,cis) 2,2-dimethyl-3-(2,2,2-trichloroethoxycarbonylethynyl)-cyclopropane-carboxylate melting at 101° C.

WORKUP

后处理

  1. stirringthe mixture was stirred for an hour
  2. filtrationhalf and filtered
  3. washThe filtrate was washed with N hydrochloric acid
  4. dry with materialwith water until neutral, dried
  5. customevaporated to dryness
  6. customThe 15.3 g of oil residue were chromatographed over silica gel
  7. washeluted with a 97-3 mixture of benzene-ethyl acetate