HRID14532

反应详情

EQUATION

反应方程式

HRID 14532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Into 3 ml of N,N-dimethylformamide was resolved 0.3 g of 4-chloro-6-(2-butynyloxy)pyrimidine, 0.57 g of potassium carbonate and 0.25 g of cis-3,5-dimethylpiperidine hydrochloride was added therein, and the mixture was stirred for 40 minutes at 70° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-buthyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.41 g of 4-(2-butynyloxy)-6-(cis-3,5-dimethylpiperidino)pyrimidine (hereinafter, referred to as Compound (23)).

WORKUP

后处理

  1. additionwas added
  2. temperatureThe reaction mixture was cooled to near room temperature
  3. extractionthe mixture was extracted with tert-buthyl methyl ether three times
  4. washThe organic layers were washed with a saturated sodium chloride aqueous solution three times
  5. dry with materialThe organic layers were dried over anhydrous magnesium sulfate
  6. concentrationconcentrated