HRID397436

反应详情

EQUATION

反应方程式

HRID 397436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

The mixture of 4-(3-chloro-4-fluoro-phenylamino)-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (90 mg, 0.32 mmol), 5-(morpholine-4-carbonyl)-thiophene-2-carbaldehyde (82 mg, 0.36 mmol), and triethylamine (2 drops) in ethanol (3 mL) was heated at 90° C. oil bath for 2 hours, and cooled to room temperature. The solvent was evaporated and the residue was purified on a silica gel column eluting with methylene chloride-methanol (98:2 and 95:5) to provide pure 4-(3-chloro-4-fluoro-phenylamino)-5-{ 1-[5-(morpholine-4-carbonyl)-thiophen-2-yl]-methylidene-}-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (41 mg, 28%). MS 486 [M++1].

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. customThe solvent was evaporated
  3. customthe residue was purified on a silica gel column
  4. washeluting with methylene chloride-methanol (98:2 and 95:5)