HRID432141

反应详情

EQUATION

反应方程式

HRID 432141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe ice-water bath was removed
  2. customreaction mixture
  3. customAcetone was removed
  4. filtrationThe solid was filtered
  5. customdried