HRID26139

反应详情

EQUATION

反应方程式

HRID 26139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4-Dichloro-β-nitrostyrene (6.6 grams, 0.030 mole) was added to a stirred solution of dimethylammonium dimethyldithiocarbamate (5.1 grams, 0.030 mole) and carbon disulfide (1.8 ml., 0.030 mole) in methanol (30 ml.). The temperature of the resulting reaction was 16-32° C. After two hours at room temperature, the precipitated product was filtered off, washed with cold methanol, and dried in air. Recrystallization without heating was accomplished by dissolving the sample in acetone and then adding absolute ethanol to give 2,4-dichloro-α-(nitromethyl)-benzyl dimethyldithiocarbamate melting at 127° C.-128° C.

WORKUP

后处理

  1. customThe temperature of the resulting reaction
  2. customwas 16-32° C
  3. filtrationthe precipitated product was filtered off
  4. washwashed with cold methanol
  5. customdried in air
  6. customRecrystallization
  7. temperaturewithout heating
  8. dissolutionby dissolving the sample in acetone
  9. additionadding absolute ethanol