HRID622074

反应详情

EQUATION

反应方程式

HRID 622074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Butyl lithium (3.9 mls of 1.14M in hexane) was added dropwise to a solution of 3-fluoroanisole (0.45 mls) in dry tetrahydrofuran (10 mls) at -75° under nitrogen. The solution was kept at -75° for 1 hour, and then acetaldehyde (0.68 mls) was added dropwise and the mixture allowed to warm up. 2M Hydrochloric acid (20 mls) was added, the mixture was extracted with ether, the organic solution was dried (MgSO4) and the solvent was evaporated. The product was distilled to give the title compound as an oil (0.4 g). NMR (CDCl3) δ 7.17 (1H, d of t, 4-H), 6.75-6.6(2H, m, 3-H, 5-H), 5.24(1H, m, CHO--), 3.89(3H, s, OCH3), 3.27 (1H, d OH), 1.56(3H, d, CH3).

WORKUP

后处理

  1. temperatureto warm up
  2. extractionthe mixture was extracted with ether
  3. dry with materialthe organic solution was dried (MgSO4)
  4. customthe solvent was evaporated
  5. distillationThe product was distilled