HRID1672567

反应详情

EQUATION

反应方程式

HRID 1672567 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of LAH (1.0 M in THF, 31 mL, 31 mmol) was added dropwise to a solution of Example 38A (5.82 g, 31.3 mmol) in THF (100 mL) at 0° C. The reaction was stirred for 1 hr, then quenched by careful addition of solid Na2SO4.10H2O. The mixture was warmed to ambient temperature and stirred 30 min. Celite filter aid was added and the mixture was filtered. The filtrate was concentrated in vacuo to yield 4.02 g (81%) of the title compound as a colorless oil. 1H NMR (300 MHz, DMSO-d6) δ 7.52 (d, J=8.2, 2H), 7.48-7.41 (m, 2H), 7.00 (t, J=56.0, 1H), 5.30 (t, J=5.7, 1H), 4.55 (d, J=5.4, 2H).

WORKUP

后处理

  1. customquenched by careful addition of solid Na2SO4.10H2O
  2. stirringstirred 30 min
  3. filtrationCelite filter aid
  4. additionwas added
  5. filtrationthe mixture was filtered
  6. concentrationThe filtrate was concentrated in vacuo