HRID1249137

反应详情

EQUATION

反应方程式

HRID 1249137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Bromomethylsaccharin (13.8 g), 1-phenyl-3-pyrazolidinone (11.9 g) and triethylamine (5.5 g) were dissolved in tetrahydrofuran (200 ml), and stirred in a stream of nitrogen at room temperature for 2 hours. The reaction mixture was added to water (200 ml), and extracted with 100 ml each of ethyl acetate two times. After drying the extract over anhydrous Glauber's salt, the solvent was distilled away. The thus obtained crude product was recrystallized from ethyl acetate to yield 16 g of N-(1-phenyl-3-pyrazolidinone-2-ylmethyl)saccharin (Compound (I)-(18)). Melting Point: 209°-213° C.

WORKUP

后处理

  1. extractionextracted with 100 ml each of ethyl acetate two times
  2. customAfter drying the
  3. extractionextract over anhydrous Glauber's salt
  4. distillationthe solvent was distilled away
  5. customThe thus obtained crude product
  6. customwas recrystallized from ethyl acetate