HRID596588
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturemaintaining the temperature at 2°-6° C
- additionAfter another 45 minutes at about 5° C. the mixture was poured into 1500 ml
- customThe precipitate was collected
- washwashed well with 5 × 500 ml
- temperatureThe dried precipitate was heated with about 200 ml
- customThe insoluble material was collected
- customrecrystallized from ethyl acetate