HRID888136

反应详情

EQUATION

反应方程式

HRID 888136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

N-(2-Acetyl-4,4-dimethyl-1,2,3,4-tetrahydro-isoquinolin-7-yl)-2-[(1H-pyrrolo[2,3-b]pyridin-6-ylmethyl)amino]nicotinamide (0.180 g, 0.384 mmol, Example 2) was dissolved into 10 mL of EtOH and 5 mL of concentrated HCl was added. The mixture was heated to 75° C. for 4 days. The volume was reduced to ⅓. Sat'd. NaHCO3 was added until the solution became cloudy. The aqueous phase was extracted with CH2Cl2 and the combined organic phases were dried over Na2SO4, filtered and concentrated to give a brown residue. The residue was purified by HPLC (Beckman) to afford the title compound. MS (ES+): 427 (M+H). Calc'd. for C25H26N6O—426.52.

WORKUP

后处理

  1. additionwas added
  2. extractionThe aqueous phase was extracted with CH2Cl2
  3. dry with materialthe combined organic phases were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give a brown residue
  7. customThe residue was purified by HPLC (Beckman)