HRID1860648
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 30 min
- customThe cooled reaction
- filtrationwas filtered through a short column of Celite®
- washwashed with ethyl acetate
- concentrationThe filtrate was concentrated