HRID1926324

反应详情

EQUATION

反应方程式

HRID 1926324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of methyl 4-[6-amino-5-(5-chloro-8-fluoroisoquinolin-3-yl)-pyridin-3-yl]-benzoate (0.13 g, 0.32 mmol) in methanol (5 mL) and water (0.5 mL) was added NaOH (0.24 g, 6 mmol), and the mixture was heated at 50° C. for 16 h. The solvents were evaporated at reduced pressure, and the residue was neutralized with acetic acid. The solid formed was filtered off and dried in vacuo to give the title compound. 1H NMR (400 MHz, DMSO-d6): δ=12.82 (very brs, 1H), 9.63 (s, 1H), 8.51 (d, J=2.4 Hz, 1H), 8.35 (s, 1H), 8.31 (d, J=2.4 Hz, 1H), 8.03-7.98 & 7.90-7.85 (AA′BB′, 4H), 7.92 (d, J=8.0 Hz, 1H), 7.27 (brs, 2H), 7.15 (d, J=8.0 Hz, 1H), 4.07 (s, 3H). MS(ES+): m/z=406.08/408.03 (100/53) [MH+]. HPLC: tR=3.00 min (polar—5 min, ZQ3).

WORKUP

后处理

  1. customThe solvents were evaporated at reduced pressure
  2. customThe solid formed
  3. filtrationwas filtered off
  4. customdried in vacuo