HRID586459

反应详情

EQUATION

反应方程式

HRID 586459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-Bromo-8-cyclopentyl-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one (1.09 g, 3.06 mmol) and 6-amino-nicotinamide (2.51 g, 18 mmol) were combined in toluene (8 ml) and heated to 100° C. for 18 hours. The mixture then was diluted with dimethylsulfoxide (8 ml) and heated to 120° C. for 2 hours. The mixture then was poured into water (120 ml) with rapid stirring. Diethyl ether was added and the resulting solid was collected by filtration. This solid was washed with 1:1 warm ethyl acetate/tetrahydrofuran and dried in vacuo to provide 6-bromo-8-cyclopentyl-2-methyl-8H-pyrido[2,3-d]pyrimidin-7-one as a yellow solid (0.233 g, 18%). MS (APCI); M++1: Calc'd, 429.06. Found, 429.1. Analyses for C18H17BrN6O2:

WORKUP

后处理

  1. temperatureheated to 120° C. for 2 hours
  2. filtrationthe resulting solid was collected by filtration
  3. washThis solid was washed with 1:1
  4. temperaturewarm ethyl acetate/tetrahydrofuran
  5. customdried in vacuo