HRID1192421
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 4-pyrido[2,3-d]pyrimidin-4-yl-piperazine-1-carboxylic acid tert-butyl ester (0.24 g, 0.76 mmol) in MeOH (10 mL) and TFA (1 mL) was added PtO2 (10 mg). The mixture was stirred under H2 (1 atm) at room temperature overnight. The catalyst was filtered off and the solvent was removed. The residue was subject to column chromatography, eluted by DCM/MeOH (20:1) to afford 4-(5,6,7,8-Tetrahydro-pyrido[2,3-d]pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester (0.15 g, 62%). 1H NMR (CDCl3, 400 MHz) δ 8.10 (s, 1H), 5.92 (s, 1H), 3.50 (m, 4H), 3.40 (m, 2H), 3.25 (m, 4H), 2.55 (m, 2H), 1.85 (m, 2H), 1.48 (s, 9H). MS (APCI+) [M+H]+320.
WORKUP
后处理
- filtrationThe catalyst was filtered off
- customthe solvent was removed
- washeluted by DCM/MeOH (20:1)