反应详情

4-[6-(8-Cyclopentyl-6-ethyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester (0.204 g, 0.39 mmol) prepared as in Example 4 was dissolved in 1:1 chloroform/methanol (16 ml) and purged with anhydrous hydrogen chloride gas. After stirring for 3.5 hours, addition of diethyl ether (8 ml) gave a solid precipitate. The solid was filtered, washed with diethyl ether and dried in vacuo yielding 0.180 g of 8-cyclopentyl-6-ethyl-2-(5-piperazin-1-yl-pyridin-2-ylamino)-8H-pyrido[2,3-d]pyrimidin-7-one hydrochloride as a yellow solid. MS (APCI); M++1: Calc'd, 420.52. Found, 420.2. Analyses for C34H29N7O.1.2H2O.2.1HCl. Calc'd: C, 53.36; H, 6.52; N, 18.93; Cl (ionic), 14.38; H2O, 4.17. Found: C, 53.25; H, 6.43; N, 18.80; Cl (ionic), 14.36; H2O, 3.87.

1. custompurged with anhydrous hydrogen chloride gas
2. additionaddition of diethyl ether (8 ml)
3. customgave a solid precipitate
4. filtrationThe solid was filtered
5. washwashed with diethyl ether
6. customdried in vacuo