HRID1011651

反应详情

EQUATION

反应方程式

HRID 1011651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 4-bromo-2-fluorobenzaldehyde (12.4 g, 61 mmol), malonic acid (12.7 g, 122 mmol) and 4-dimethylamino pyridine (0.75 g, 6.1 mmol) in 20 mL of DMF was heated at 100 degrees Celsius for 2 hrs. After cooling, the reaction mixture was diluted with 300 mL water, and filtered. The solid was collected, and triturated in hexane. The solid was collected and dried in vacuum to give 12.7 g (85%) of a white solid. MS: calc'd 243 (M−H), exp 243 (M−H).

WORKUP

后处理

  1. temperaturewas heated at 100 degrees Celsius for 2 hrs
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. customThe solid was collected
  5. customtriturated in hexane
  6. customThe solid was collected
  7. customdried in vacuum