HRID1032990

反应详情

EQUATION

反应方程式

HRID 1032990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-amino-5-ethyl-6-methyl-2-(1H)-pyridinone (152 mg, 1.0 mmol), 2-chloromethyl-1,3-benzthiazole (184 mg, 1.0 mmol) and triethylamine (0.14 mL, 1.0 mmol) in absolute ethanol (5 mL) was stirred at reflux for 24 hours. After filtering and concentrating under reduced pressure, the residue was flash chromatographed over silica gel. Elution with 4% MeOH- 96% CHCl3 gave 233 mg of product. Recrystallization from EtOH-water gave 77 mg of analytically pure product, mp 209°-210° C. Anal. Calcd for C16H17N3OS: C, 67.83; H, 6.05; N, 14.83. Found: C, 67.71; H, 6.03; N, 14.70.

WORKUP

后处理

  1. temperatureat reflux for 24 hours
  2. filtrationAfter filtering
  3. concentrationconcentrating under reduced pressure
  4. customchromatographed over silica gel
  5. washElution with 4% MeOH- 96% CHCl3