HRID1182705

反应详情

EQUATION

反应方程式

HRID 1182705 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Butyl-5-hydroxyisoindolin-1-one (366 mg, 1.78 mmol), K2CO3 (493 mg, 3.57 mmol) and KI (296 mg, 1.78 mmol) were added to a solution of (2,6-dimethyl-4-phenylpyridin-3-yl)methyl methanesulfonate (520 mg, 1.78 mmol) in DMF (18 mL). After stirring overnight at room temperature (rt), water was added and the pH was adjusted to 13-14 using aqueous NaOH (1 M). The reaction mixture was extracted with EtOAc, the combined organic layers were washed with water, dried with MgSO4 and the solvent was removed in vacuo. Purification by flash chromatography (DCM/MeOH, gradient 1-5% MeOH) provided 2-butyl-5-((2,6-dimethyl-4-phenylpyridin-3-yl)methoxy)isoindolin-1-one (140 mg, 19%). ESI-MS [M+H]+=401.2.

WORKUP

后处理

  1. additionwas added
  2. extractionThe reaction mixture was extracted with EtOAc
  3. washthe combined organic layers were washed with water
  4. dry with materialdried with MgSO4
  5. customthe solvent was removed in vacuo
  6. customPurification by flash chromatography (DCM/MeOH, gradient 1-5% MeOH)