HRID224649

反应详情

EQUATION

反应方程式

HRID 224649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-[[5-[(methylamino)methyl]-2-furanylmethyl]thio]ethanamine (6.0 g) and 1,1-bis-(methylthio)-2-nitroethane (19.8 g) in dry dimethylformamide (150 ml) was stirred for 1 hour at 0° and for 5 hours at room temperature. A solution of oxalic acid (4.0 g) in dry dimethylformamide (16 ml) was added and the solid which formed during 18 hours was filtered, washed with dimethylformamide, ethanol and ether and dried. The solid was suspended in water (200 ml) at 55° and on cooling was filtered, washed with water and dried to give the title compound (3.25 g) m.p. 158°-160° dec.

WORKUP

后处理

  1. customthe solid which formed during 18 hours
  2. filtrationwas filtered
  3. washwashed with dimethylformamide, ethanol and ether
  4. customdried
  5. customwas suspended in water (200 ml) at 55°
  6. temperatureon cooling
  7. filtrationwas filtered
  8. washwashed with water
  9. customdried