HRID1798693

反应详情

EQUATION

反应方程式

HRID 1798693 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methanesulfonic acid (531 mg, 5.5 mmol) was added to a solution of 4-(4-(imidazo[1,2-a]pyridin-2-ylmethoxy)phenyl)-5-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one (2.5 g, 5.5 mmol) in DCM (5 ml) and diethyl ether (150 mL) at RT under an atmosphere of nitrogen. The reaction mixture was stirred for a further 4 h at RT. The solids were collected by filtration, washed with 20% DCM in diethyl ether and dried in vacuo to afford 4-(4-(imidazo[1,2-a]pyridin-2-ylmethoxy)phenyl)-5-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one methanesulfonate (2.4 g, 82.7%) as white solid. 1H NMR: 500 MHz, DMSO-d6: δ 8.75 (d, 1H), 8.1 (s, 1H), 7.65 (Ar, 3H), 7.3-6.85 (Ar, 8H), 5.2 (s, 2H), 3.85 (s, 3H), 1.25 (s, 6H), HPLC: (98.8%, Condition-A).

WORKUP

后处理

  1. filtrationThe solids were collected by filtration
  2. washwashed with 20% DCM in diethyl ether
  3. customdried in vacuo