HRID857431

反应详情

EQUATION

反应方程式

HRID 857431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

1.14 g of 3,5-dichloroaniline (10 mmol), 0.97 g of glyoxylic acid hydrate (15 mmol) and 1.40 g of cyclopentadiene (freshly distilled) (30 mmol) were dissolved in 20 ml of acetonitrile in a closable Teflon vessel and heated to 50° C. within one minute in a microwave oven with a power of 800 watts and kept at this temperature for five minutes with further microwave irradiation. The vessel was then placed in ice water, cautiously opened and evaporated in a rotary evaporator. The mass of crystals obtained was washed with hexane and dried. A colourless mass of crystals was obtained in a quantity of 1.95 g (98% of theoretical).

WORKUP

后处理

  1. customkept at this temperature for five minutes with further microwave irradiation
  2. customevaporated in a rotary evaporator
  3. customThe mass of crystals obtained
  4. washwas washed with hexane
  5. customdried
  6. customA colourless mass of crystals was obtained in a quantity of 1.95 g (98% of theoretical)