HRID654098

反应详情

EQUATION

反应方程式

HRID 654098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-(3-chloropropyl)-5,6-dihydro-(1H,4H)-1,2,5-thiadiazolo[4,3,2-ij]quinoline 2,2-dioxide (4 g), 4-(4-hydroxyphenyl)piperazine (4.75 g) and triethylamine (5.88 cc) in dry N,N-dimethylformamide (50 cc) is heated to reflux for 90 minutes and is then cooled and poured into a mixture of water (300 cc) and ethyl acetate (300 cc). The organic phase is washed with water (3×200 cc), is dried over magnesium sulphate and is concentrated to dryness under reduced pressure (2.7 kPa). The solid is recrystallized from ethyl acetate (300 cc) and dried. 1-[3-(4-(4-Hydroxyphenyl)-1-piperazinyl)propyl]-5,6-dihydro(1H,4H)-1,2,5-thiadiazolo[4,3,2-ij]quinoline 2,2-dioxide (2.8 g) is obtained, melting at 182° C.

WORKUP

后处理

  1. temperatureto reflux for 90 minutes
  2. temperatureis then cooled
  3. washThe organic phase is washed with water (3×200 cc)
  4. dry with materialis dried over magnesium sulphate
  5. concentrationis concentrated to dryness under reduced pressure (2.7 kPa)
  6. customThe solid is recrystallized from ethyl acetate (300 cc)
  7. customdried