HRID2232236

反应详情

EQUATION

反应方程式

HRID 2232236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Hydroxy-3-(4-methoxyphenyl)-1,2,4-triazolo[3,4-a]phthalazine, (9.8 g), is suspended in N,N-dimethylformamide (100 ml) and added of 50% sodium hydride in mineral oil (1.7 g). The mixture is heated to 50°-60° C. and stirred for about 2 hours. After cooling to room temperature the mixture is added portionwise with 3-bromo-2-pyrrolidone (5.5 g). [This product is prepared according to F. Korte, H. Wanholf, Ber. 97, 1976 (1964)]. Then stirring is continued for about 5 hours at a temperature of about 70° C. The mixture is then cooled to room temperature and poured into water (800 ml). The residue, which is collected by filtration, is then crystallized from ethanol/chloroform. (Yield=82%). M.p. 290°-293° C.

WORKUP

后处理

  1. temperatureThe mixture is heated to 50°-60° C.
  2. custom[This product is prepared
  3. stirringThen stirring
  4. waitis continued for about 5 hours at a temperature of about 70° C
  5. temperatureThe mixture is then cooled to room temperature
  6. filtrationThe residue, which is collected by filtration
  7. customis then crystallized from ethanol/chloroform