HRID2250390

反应详情

EQUATION

反应方程式

HRID 2250390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

300 mg of 3-[4-methyl-6-(trityl-amino)-pyridin-2-yl]propionic acid (compound C4) and 156 mg of 2,3-diamino-5-(4-chlorophenyl)-pyridine (compound F4) are dissolved in 13 ml of pyridine and sequentially treated with 280 mg of O-[(ethoxycarbonyl)canomethylene-amino]-N,N,N′,N′-tetramethyl-uronium tetrafluoroborate and 153 μl of diisopropylethyl amine. The reaction mixture is warmed to 40° C. for 120 h. Purification of the crude product by chromatography on silica gel (eluent: dichloromethane/methanol 8:1) afforded 405 mg of the title compound as an oil. ESI-MS: 624.1/626.1 (MH+, 100%/38%). TLC: Rf=0.32 (dichloromethane/methanol 8:1).

WORKUP

后处理

  1. customPurification of the crude product by chromatography on silica gel (eluent: dichloromethane/methanol 8:1)