HRID1935319
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
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
- customexcess BCl3 and CH2Cl2 were removed
- washThe resulting material was washed with CH2Cl2
- customThe product was obtained as a white powder in 62% yield