HRID1077334

反应详情

EQUATION

反应方程式

HRID 1077334 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

49.6 g of a crude 5-nitronaphthoquinone cake (which had a water content of 50 wt% and a dry weight of 24.8 g, and comprised of 82 wt% of 5-nitronaphthoquinone and 10 wt% of 6-nitronaphthoquinone when determined under dried condition by a gas chromatography), 12.1 g of 1,3-butadiene and 49.6 g of benzene were introduced into an autoclave, which was then hermetically sealed for reaction at 80°C for 2.5 hours. The resultant reaction solution was cooled to 25°-30°C to crystalize 5-nitrotetrahydroanthraquinone, subjected to filtration, washed with 40 g of methanol, and dried to obtain 22.4 g of 5-nitrotetrahydroanthraquinone. The yield was 87.0% of the theoretical (based on the 5-nitronaphthoquinone contained in the crude starting material).

WORKUP

后处理

  1. dry with materialunder dried condition by a gas chromatography), 12.1 g of 1,3-butadiene and 49.6 g of benzene
  2. additionwere introduced into an autoclave, which
  3. customwas then hermetically sealed for reaction at 80°C for 2.5 hours
  4. customThe resultant reaction solution
  5. temperaturewas cooled to 25°-30°C
  6. customto crystalize 5-nitrotetrahydroanthraquinone
  7. filtrationsubjected to filtration
  8. washwashed with 40 g of methanol
  9. customdried