HRID712471

反应详情

EQUATION

反应方程式

HRID 712471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of tert-butyl 2-(3-((4-((3-chloro-4-fluorophenyl)amino)-7-methoxyquinazolin-6-yl)oxy) propyl)hexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H)-carboxylate (0.40 g) in CH2Cl2 was added a solution of HCl in EtOAc (3 M, 10 mL). White solid was precipitated out after 2 h reaction. The resulted mixture was filtered and the residue was dried to give the title compound as a pale yellow solid (0.30 g, 80.00%), HPLC: 99.00%. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 486.2 (M+1); 1H NMR (400 MHz, D2O) δ: 1.97-2.03 (m, 4H), 2.68-2.71 (m, 2H), 2.80-2.86 (m, 4H), 2.87-2.91 (m, 2H), 3.40-3.45 (m, 2H), 4.07-4.11 (m, 2H), 4.19 (s, 3H), 4.39-4.43 (m, 2H), 7.441 (s, 1H), 7.50 (t, J=8.6 Hz, 1H), 7.84 (s, 2H), 8.68 (t, J=4.6 Hz, 1H), 8.89 (s, 1H) ppm.

WORKUP

后处理

  1. customWhite solid was precipitated out after 2 h
  2. customreaction
  3. filtrationThe resulted mixture was filtered
  4. customthe residue was dried