HRID70735

反应详情

EQUATION

反应方程式

HRID 70735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaH (60% in mineral oil, 1.2 g, 30 mmol) was added to an ice-cooled solution of (4-hydroxy-phenyl)-phenyl-methanone (5 g, 25.2 mmol) in DMF (25 mL). Stirred for 20 minutes at room temperature. Benzyl bromide (6.1 ml, 50 mmol) was added at 0° C. The reaction temperature was raised to room temperature after 1 h. Stirred 2 h. Water (20 mL) was added and aqueous phase was extracted dichloromethane (2×30 mL). The combined organic phase was concentrated and purified by flash chromatography (eluent: dichloromethane). 1H nmr revealed the product was pure. Yield: 7.0 g, 96%

WORKUP

后处理

  1. temperatureThe reaction temperature was raised to room temperature after 1 h
  2. stirringStirred 2 h
  3. extractionaqueous phase was extracted dichloromethane (2×30 mL)
  4. concentrationThe combined organic phase was concentrated
  5. custompurified by flash chromatography (eluent: dichloromethane)