HRID1503479
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 microwave vial equipped with a magnetic stirrer was charged with 6,6-dimethyl-6,7-dihydro-4H-pyrazolo[5,1-c][1,4]oxazin-3-amine (13 mg, 0.078 mmol), 2-chloro-N-methyl-5-(trifluoromethyl)pyrimidin-4-amine (20 mg, 0.095 mmol), and t-BuOH (0.5 mL). The mixture was heated at 100° C. under microwave irradiation for 15 min. After concentration, the residue was purified by prep-HPLC to give the title compound (9.5 mg, 36%). 1H NMR (500 MHz, CDCl3) δ 8.09 (s, 1H), 7.67 (s, 1H), 6.79 (s, 1H), 5.18 (s, 1H), 4.83 (s, 2H), 3.93 (s, 2H), 3.00 (d, J=4.5 Hz, 3H), 1.63 (s, 6H). LC-MS (Method B): m/z=343.3 (M+H)+, 4.77 min, 98.2% purity.
WORKUP
后处理
- customA microwave vial equipped with a magnetic stirrer
- concentrationAfter concentration
- customthe residue was purified by prep-HPLC