反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 95 °C
PROCEDURE
实验过程
A suspension of 3-Amino-1-[4-(4-dimethylamino-phenyl)-pyrimidin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (250 mg, 0.71 mM) in 1 N KOH (3 ml) and MeOH (4 ml) was heated at 95° C. for 1 hr allowing some methanol to distil off. The reaction was cooled to room temperature and neutralized with 1 N HCl. The resulting precipitate was collected via filtration, washed with water (1×3 ml) and then dried in vacuo overnight to afford 3-Amino-1-[4-(4-dimethylamino-phenyl)-pyrimidin-2-yl]-1H-pyrazole-4-carboxylic acid (170 mg, 73% yield) as a yellow solid. ES-MS MH+325.4 1H NMR (300 MHz, ppm, DMSO-d6): 8.72 (s, 1H), 8.60 (d, 1H), 8.15 (d, 2H), 7.70 (d, 1H), 6.82 (d, 2H), 5.77 (br, 2H), 3.03 (s, 6H)
WORKUP
后处理
- customto distil off
- temperatureThe reaction was cooled to room temperature and neutralized with 1 N HCl
- filtrationThe resulting precipitate was collected via filtration
- washwashed with water (1×3 ml)
- customdried in vacuo overnight