HRID1016461

反应详情

EQUATION

反应方程式

HRID 1016461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 7-chloro-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (3.0 g, 16.5 mmol) in ethanol (60 mL) was added ethylene diamine (4 mL, 60 mmol). After refluxing 18 hours the reaction was cooled, poured into saturated aqueous sodium bicarbonate, and then washed with ethyl acetate. The aqueous layer was then extracted with 3:7 isopropyl alcohol/chloroform, the combined extracts were dried (Na2SO4) and then concentrated under reduced pressure to give the title compound as an amorphous brown solid (3.2 g, 94%): +APcI MS (M+1)+ 206; 1H NMR (methanol-d4) δ: 6.05 (s, 1H), 6.00 (s, 1H), 3.45 (m, 2H), 2.91 (m, 2H).

WORKUP

后处理

  1. temperatureAfter refluxing 18 hours the reaction
  2. temperaturewas cooled
  3. washwashed with ethyl acetate
  4. extractionThe aqueous layer was then extracted with 3:7 isopropyl alcohol/chloroform
  5. dry with materialthe combined extracts were dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure