HRID1050720

反应详情

EQUATION

反应方程式

HRID 1050720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.8 g of lithium aluminum hydride and 20 mL of tetrahydrofuran were added in a 150 mL of single-neck flask equipped with a magnetic stirrer. After stirred for 0.5 to 1.0 hour under ice bath cooling, 1.5 g of N-ethyl-2,4-dimethylthiazole-5-carboxamide in 10 mL of tetrahydrofuran solution are added dropwise, and reacted at the same temperature for 0.5 to 10 hours, and then for 1 to 2 hours at room temperature. The reaction mixture was then extracted with ethyl acetate, the organic layer was separated while the aqueous layer was extracted with ethyl acetate twice. The organic phases were combined, and dried over anhydrous sodium sulfate after washed with an iced aqueous sodium chloride solution twice, then remove the solvent under reduced pressure to obtain 1.0 g of 2,4-dimethyl-5-ethylaminomethylthiazole which was used in the next step directly without purification.

WORKUP

后处理

  1. customequipped with a magnetic stirrer
  2. temperaturecooling
  3. customreacted at the same temperature for 0.5 to 10 hours
  4. waitfor 1 to 2 hours at room temperature
  5. extractionThe reaction mixture was then extracted with ethyl acetate
  6. customthe organic layer was separated while the aqueous layer
  7. extractionwas extracted with ethyl acetate twice
  8. dry with materialdried over anhydrous sodium sulfate
  9. washafter washed with an iced aqueous sodium chloride solution twice
  10. customremove the solvent under reduced pressure