HRID2379167

反应详情

EQUATION

反应方程式

HRID 2379167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Bromosuccinimide (0.90 g, 5.06 mmol) was added to a stirred solution of the compound from Step 2 (1.04 g, 4.60 mmol) in CCl4 (150 ml) followed by a catalytic amount of azobis (isobutyronitrile). After the mixture was refluxed for 3 h., the precipitated solid was removed by filtration and the solvent was evaporated in vacuo. The residue was stirred for 10 min. in 15 ml Et2O, filtered and dried to give 0.69 g of the title compound, m.p. 155°-156° C.

WORKUP

后处理

  1. temperatureAfter the mixture was refluxed for 3 h.
  2. customthe precipitated solid was removed by filtration
  3. customthe solvent was evaporated in vacuo
  4. filtrationfiltered
  5. customdried