HRID1873216
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 suspension of 2-benzofuranylphenyl-methanone (34.8 g, 0.157 mol), hydrazine monohydrate (31 mL, 0.639 mol) and diethylene glycol (72 mL) was heated to reflux for 10 min and cooled to room temperature. Potassium hydroxide (22.9 g, 0.408 mol) was added. The reaction mixture was heated in 130° C. oil bath for 1 h., cooled to room temperature and added to water. The oil was extracted with ether. Silica ge was added to the ether phase and the solvent was removed. The adsorbate was flash chromatographed eluent: (petroleum ether) to provide the title compound as an oil (23.9 g, 90%): NMR (CDCl3); δ7.5-7.1 (m, 9 H), 6.38 (s, 1 H), 4.10 (s, 2 H).
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 10 min
- temperatureThe reaction mixture was heated in 130° C. oil bath for 1 h.
- temperaturecooled to room temperature
- extractionThe oil was extracted with ether
- additionSilica ge was added to the ether phase
- customthe solvent was removed
- customchromatographed eluent