HRID596588

反应详情

EQUATION

反应方程式

HRID 596588 的结构方程式

CONDITIONS

反应条件

温度
2 °C

PROCEDURE

实验过程

Fuming red nitric acid (150 ml.) was cooled to 2° C. and 27.3 g. of 5,6,7,8-tetrahydronaphthalene-1-carboxylic acid was added portionwise over 0.5 hour with stirring maintaining the temperature at 2°-6° C. After another 45 minutes at about 5° C. the mixture was poured into 1500 ml. of crushed ice. The precipitate was collected and washed well with 5 × 500 ml. portions of water. The dried precipitate was heated with about 200 ml. of benzene. The insoluble material was collected and recrystallized from ethyl acetate to give 3-nitro-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid, m.p. 209°-212° C.

WORKUP

后处理

  1. temperaturemaintaining the temperature at 2°-6° C
  2. additionAfter another 45 minutes at about 5° C. the mixture was poured into 1500 ml
  3. customThe precipitate was collected
  4. washwashed well with 5 × 500 ml
  5. temperatureThe dried precipitate was heated with about 200 ml
  6. customThe insoluble material was collected
  7. customrecrystallized from ethyl acetate