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
- 0 °C
PROCEDURE
实验过程
1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (Compound 9) (3.80 g, 8.57 mmol) was suspended in 190 ml of acetone and cooled to 0° C. 48 ml of 5.0N hydrochloric acid was added slowly through an additional funnel. The ice-water bath was removed and reaction mixture was stirred at room temperature overnight. Acetone was removed and aqueous layer was neutralized with 1.0N sodium hydroxide to PH about 10. The solid was filtered and dried to give 2.926 g of 4-(4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-1-cyclohexanone. 1H NMR (CDCl3) 2.39 (m, 2H), 2.62 (m, 6H), 5.3 0 (m, 1H), 6.08 (bs, 2H), 7.09 (m, 2H), 7.15 (m, 3H), 7.42 (m, 2H), 7.64 (d, J=8.70 Hz, 2H), 8.39 (s, 1H); LC/MS (MH+=400).
WORKUP
后处理
- customThe ice-water bath was removed
- customreaction mixture
- customAcetone was removed
- filtrationThe solid was filtered
- customdried