HRID2261189
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
- 120 °C
PROCEDURE
实验过程
Acetic anhydride (0.123 mL, 1.3 mmol) is added to (3-(9-ethyl-8-imino-8,9-dihydro-3H-3,4,9-triaza-cyclopenta[a]naphthalen-7-yl)-5-methoxy-benzoic acid ethyl ester (100 mg, 0.26 mmol) in sealed tube and heated at 120° C. for 2.5 hr. The acetic anhydride is evaporated and 6N HCl (3 mL) is added and the mixture is again heated at 105° C. for 1 hr. The reaction mixture is brought to room temperature and poured in ice cold water. The acid is crystallized out and filtered. It is washed with water and dried to give the desired product. MS m/z 364.2 (M+1).
WORKUP
后处理
- customThe acetic anhydride is evaporated
- addition6N HCl (3 mL) is added
- temperaturethe mixture is again heated at 105° C. for 1 hr
- customis brought to room temperature
- additionpoured in ice cold water
- customThe acid is crystallized out
- filtrationfiltered
- washIt is washed with water
- customdried