HRID1935319

反应详情

EQUATION

反应方程式

HRID 1935319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of compound 17 (238 milligrams, 0.492 millimoles) in CH2Cl2 was added 1.97 milliliters of 1 molar BCl3 (1.97 millimoles) in CH2Cl2. After 30 minutes, excess BCl3 and CH2Cl2 were removed by passing a stream of nitrogen gas across the surface of the solution. The resulting material was washed with CH2Cl2. The product was obtained as a white powder in 62% yield. TLC (4:1:1 n-butanol:acetic acid:water) indicated a single spot that was also UV active (Rf=0.47). 1H-NMR (DMSO): δ7.6-7.8 (m, 3H), 8.0-8.15 (m, 1H), 10.25 (brs.).

WORKUP

后处理

  1. customexcess BCl3 and CH2Cl2 were removed
  2. washThe resulting material was washed with CH2Cl2
  3. customThe product was obtained as a white powder in 62% yield