HRID1666066

反应详情

EQUATION

反应方程式

HRID 1666066 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 2-chloro-6-[(2,2-dimethyl-propyl)-amino]-5-fluoro-nicotinonitrile (150 mg, 0.62 mmol), 3-amino-N-methoxy-4-methyl-benzamide (150 mg, 0.83 mmol) and potassium fluoride (30 mg, 0.51 mmol) in DMSO (1 mL) was heated to 150° C. overnight. The reaction mixture was allowed to cool to room temp and then partitioned between water and ethyl acetate. The organic layer was dried (sodium sulfate) and concentrated under reduced pressure. The product (2.5 mg, 1%) was obtained after purification by silica gel chromatography with 30% EtOAc in hexane as eluent. C20H24FN5O2 MS m/e=386 (M+H).

WORKUP

后处理

  1. temperatureto cool to room temp
  2. custompartitioned between water and ethyl acetate
  3. dry with materialThe organic layer was dried (sodium sulfate)
  4. concentrationconcentrated under reduced pressure