HRID1860648

反应详情

EQUATION

反应方程式

HRID 1860648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of the product from STEP 9 (335 mg), iron powder (74 mg, 1.3 mmol), triphenylphosphine (236 mg, 0.9 mmol), and acetic acid (6.3 ml) was heated at reflux for 30 min. The cooled reaction was filtered through a short column of Celite®, and washed with ethyl acetate. The filtrate was concentrated to give 108 mg of an colorless oil. This product mixture was used without further purification. The 1H NMR spectrum of the product was consistent for the proposed structure.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 30 min
  3. customThe cooled reaction
  4. filtrationwas filtered through a short column of Celite®
  5. washwashed with ethyl acetate
  6. concentrationThe filtrate was concentrated