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
- 100 °C
PROCEDURE
实验过程
A mixture of 3-Amino-1-(8-methoxy-5,6-dihydro-benzo[h]quinazolin-2-yl)-1H-pyrazole-4-carboxylic acid ethyl ester(3, 3.15 g, 8.63 mM), 1 N NaOH (15 mL), and methanol (20 mL) was heated at 100° C. for 3 hr then cooled to room temperature and diluted with water (100 mL). the pH was adjusted with 1 N HCl to approximately 3-4 and the resulting precipitate was isolated via filtration, washed with water (2×80 mL) and dried in vaccuo to give 3-Amino-1-(8-methoxy-5,6-dihydro-benzo[h]quinazolin-2-yl)-1H-pyrazole-4-carboxylic acid (4, 3.02 g, 100% yield). ES-MS MH+ 338.4 1H NMR (300 MHz, ppm, DMSO-d6): 8.81 (s, 1H), 8.57 (s, 1H), 8.2 (d, 1H), 7.0 (dd, 1H), 6.95 (s, 1H), 3.85 (s, 3H), 2.93 (m, 4H).
WORKUP
后处理
- temperaturethen cooled to room temperature
- customthe resulting precipitate was isolated via filtration
- washwashed with water (2×80 mL)
- customdried in vaccuo