HRID559186

反应详情

EQUATION

反应方程式

HRID 559186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-[3-(4-bromophenyl)-1,9-dimethyl-2-oxo-2,9-dihydro-1H-pyrido[2,3-b]indol-6-yl]-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester are dissolved in 5 ml of anhydrous CH2Cl2 anhydrous. The mixture is refluxed and then 0.2 ml of 1M LiBH4 in THF is added. The mixture is refluxed for 20 hours, while further adding 3 times 0.2 ml of LiBH4. The mixture is allowed to return to ambient temperature and 1 ml of 2N NaOH is added. The reaction medium is evaporated to dryness. Water is added, and the medium is acidified with 1N HCl and extracted with EtOAc. The organic phase is evaporated to dryness. The product is triturated in water, filtered, and washed with water. The product is taken up in methanol and evaporated to dryness.

WORKUP

后处理

  1. temperatureThe mixture is refluxed
  2. temperatureThe mixture is refluxed for 20 hours
  3. customto return to ambient temperature
  4. customThe reaction medium is evaporated to dryness
  5. additionWater is added
  6. extractionextracted with EtOAc
  7. customThe organic phase is evaporated to dryness
  8. customThe product is triturated in water
  9. filtrationfiltered
  10. washwashed with water
  11. customevaporated to dryness