HRID2261189

反应详情

EQUATION

反应方程式

HRID 2261189 的结构方程式

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

  1. customThe acetic anhydride is evaporated
  2. addition6N HCl (3 mL) is added
  3. temperaturethe mixture is again heated at 105° C. for 1 hr
  4. customis brought to room temperature
  5. additionpoured in ice cold water
  6. customThe acid is crystallized out
  7. filtrationfiltered
  8. washIt is washed with water
  9. customdried