HRID643340

反应详情

EQUATION

反应方程式

HRID 643340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-benzyl-8-trifluoromethyl-cinnolin-4-ol (1.6 g, 4.4 mmol) and POBr3 (2.5 g, 8.7 mmol) in DMF (30 ml) was heated to 75° C. After 1 hr, the reaction was cooled and poured into water. The aqueous layer was extracted with EtOAc which was dried (MgSO4) and concentrated to give a solid. The solid was triturated with MeOH and filtered to give 3-benzyl-4-bromo-8-trifluoromethyl-cinnoline (1.7 g). MS (ES) m/z 366.7.

WORKUP

后处理

  1. temperaturethe reaction was cooled
  2. extractionThe aqueous layer was extracted with EtOAc which
  3. dry with materialwas dried (MgSO4)
  4. concentrationconcentrated
  5. customto give a solid
  6. customThe solid was triturated with MeOH
  7. filtrationfiltered