HRID2067319

反应详情

EQUATION

反应方程式

HRID 2067319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 2-amino-4-methylthiazole-5-carboxylate (0.50 g, 2.68 mmol) and pyridine (0.32 mL, 4.03 mmol) in tetrahydrofuran (25 mL) and dichloromethane (25 mL) was added 4-nitrophenyl chloroformate (0.65 g, 3.22 mmol) at 0° C. The resulting reaction mixture was stirred at ambient temperature for 1 hour, followed by the addition of hydrazine monohydrate (3.00 mL, 59.9 mmol). The reaction mixture was stirred at ambient temperature for 18 hours and quenched with water (100 mL). The solid precipitated was filtered, washed with water and ethyl acetate and dried to afford the title compound in 78% yield (0.51 g): MS (ES+) m/z 245.2 (M+1).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. stirringThe reaction mixture was stirred at ambient temperature for 18 hours
  3. customquenched with water (100 mL)
  4. customThe solid precipitated
  5. filtrationwas filtered
  6. washwashed with water and ethyl acetate
  7. customdried