HRID1027902

反应详情

EQUATION

反应方程式

HRID 1027902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Example 118A (170 mg, 0.7 mmol) in methanol (15 mL) was treated with Raney nickel (slurry in H2O, 1 spatula) and refluxed for 16 hours. The mixture was filtered through diatomaceous earth and washed with methanol. The filtrate was concentrated under vacuum to provide the title compound. 1H NMR (CD3OD) δ 2.24 (t, 2H), 2.40 (t, 2H), 2.59 (t, 2H), 7.27-7.34 (m, 1H), 7.36-7.42 (m, 2H), 7.60-7.66 (m, 1H), 8.14-8.18 (m, 1H). MS (M+H)+ m/z 213

WORKUP

后处理

  1. temperaturerefluxed for 16 hours
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. washwashed with methanol
  4. concentrationThe filtrate was concentrated under vacuum