HRID493709

反应详情

EQUATION

反应方程式

HRID 493709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 4-(((2Z)-3-methyl-2-methylimino-2,3-dihydro-1,3-thiazol-4-yl)methyl)piperazine-1-carboxylate (1.0 g) obtained in Example 11a) was dissolved in THF (20 mL), n-butyllithium (4.6 mL; a 1.6 M hexane solution) was added thereto at −70° C., and the mixture was mixed for 30 minutes. To the reaction solution was added DMF (1.0 mL), mixed at −70° C. for 1 hour, and then an aqueous ammonium chloride solution was added thereto at 0° C. The mixture was extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off to give the title compound (1.1 g) as a pale brown oily matter.

WORKUP

后处理

  1. additionat −70° C., and the mixture was mixed for 30 minutes
  2. additionmixed at −70° C. for 1 hour
  3. customat 0° C
  4. extractionThe mixture was extracted with ethyl acetate
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off