HRID1366605

反应详情

EQUATION

反应方程式

HRID 1366605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Tris(1,1-dimethylethyl)2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate (1.16 g, 2.339 mmol) was dissolved in THF (5 mL). To this solution was added triethylamine (0.39 mL, 2.8 mmol), followed by N-methyl-1-(1,3-thiazol-2-yl)methanamine (0.30 g, 2.3437 mmol) in THF (2 mL). The reaction was left to stir overnight. Then the reaction mixture was diluted with water, and the aqueous layer was extracted with ethyl acetate. The organics were dried (Na2SO4) and concentrated to produce tris(1,1-dimethylethyl)2-{2-chloro-5-fluoro-6-[methyl(1,3-thiazol-2-ylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate as a white solid (1.51 g). LCMS: (M+H−Boc)+=489.1.

WORKUP

后处理

  1. waitThe reaction was left
  2. extractionthe aqueous layer was extracted with ethyl acetate
  3. dry with materialThe organics were dried (Na2SO4)
  4. concentrationconcentrated