HRID914387

反应详情

EQUATION

反应方程式

HRID 914387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of {2-[(2-tert-butoxy-1,1-dimethyl-2-oxoethyl)thio]-1,3-thiazol-4-yl}acetic acid (160 g) obtained in Example 3 in dichloromethane (500 mL) were added 9H-fluorene-9-ylmethanol (98 g) and 4-dimethylaminopyridine (3.1 g), diisopropylcarbodiimide (78 ml) was added dropwise under ice-cooling, and the mixture was stirred at 0° C. for 1 hr and further stirred at room temperature for 2 hr. The precipitate was removed from the reaction mixture by filtration, and the filtrate was concentrated under reduced pressure and purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=4:1) to give the title compound (260 g) as a yellow oil.

WORKUP

后处理

  1. additionwas added dropwise under ice-
  2. temperaturecooling
  3. stirringfurther stirred at room temperature for 2 hr
  4. customThe precipitate was removed from the reaction mixture by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. custompurified by silica gel chromatography (elution solvent; hexane:ethyl acetate=4:1)