HRID594983
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
- 180 °C
PROCEDURE
实验过程
1-((6-fluoropyridin-2-yl)methyl)-N-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-amine (Example 170) (45 mg, 0.138 mmol) was dissolved in DMF (0.6 ml) in a microwave tube under Nitrogen. This was sealed and heated at 180° C. for 1 h. The mixture was concentrated and purified by prep HPLC to afford 1-46-(dimethylamino)pyridin-2-yl)methyl)-N-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-amine as yellowish solid (20 mg, 42% yield). 1H NMR (d6-Acetone) δ 8.88 (s and br s, 2H), 8.06 (s, 1H), 7.99 (s, 1H), 7.61 (s, 1H), 7.40 (t, 1H), 6.49 (d, 1H), 6.24 (br s, 1H), 5.51 (s, 2H), 3.83 (s, 3H), 3.02 (s, 6H); LC-MS method B, (ES+) 350.1, RT=5.06 min.
WORKUP
后处理
- customThis was sealed
- concentrationThe mixture was concentrated
- custompurified by prep HPLC