HRID272431

反应详情

EQUATION

反应方程式

HRID 272431 的结构方程式

PROCEDURE

实验过程

4-[6-(8-Cyclopentyl-6-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester (0.411 g, 0.813 mmol), prepared as in Example 19, was dissolved in a 1:1 mixture of methanol/chloroform, purged with anhydrous hydrogen chloride gas, stirred for 2 hours at room temperature and a solid precipitated by addition of diethyl ether. The suspension was filtered and the residue dried in vacuo yielding 8-cyclopentyl-6-methyl-2-(5-piperazin-1-yl-pyridin-2-ylamino)-8H-pyrido[2,3-d]pyrimidin-7-one hydrochloride as a yellow solid (0.393 g). (APCI); M++1: Calc'd, 406.50. Found, 406.2. Analyses for C22H27N7O.2.85H2O.2.2HCl: Calc'd: C, 49.20; H, 6.55; N, 18.26, Cl (ionic), 14.52; H2O, 9.56 Found: C, 49.43; H, 6.32; N, 17.87; Cl (ionic), 14.38 ; H2O, 7.35

WORKUP

后处理

  1. custompurged with anhydrous hydrogen chloride gas
  2. customa solid precipitated by addition of diethyl ether
  3. filtrationThe suspension was filtered
  4. customthe residue dried in vacuo