HRID29884

反应详情

EQUATION

反应方程式

HRID 29884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

A mixture of piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide hydrochloride (2.51 g, 7.16 mmol) and 4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (1.00 g, 5.97 mmol) in iso-propanol (15 mL) was placed in a microwave vessel, followed by addition of triethylamine (2.5 mL, 18 mmol). The microwave vessel was sealed then heated in the microwave at normal absorbance at 190° C. for 60 min. The mixture was concentrated to remove most of the iso-propanol and triethylamine. The residue was washed with methanol (2×15 mL) to afford a brown solid. The solid was washed with water (3×30 mL) and dried overnight to afford 1-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide (1.83 g, 69%) as a light-brown solid ((M+H)+: 446.3).

WORKUP

后处理

  1. customwas placed in a microwave vessel
  2. customThe microwave vessel was sealed
  3. concentrationThe mixture was concentrated
  4. customto remove most of the iso-propanol and triethylamine
  5. washThe residue was washed with methanol (2×15 mL)
  6. customto afford a brown solid
  7. washThe solid was washed with water (3×30 mL)
  8. customdried overnight