HRID480453

反应详情

EQUATION

反应方程式

HRID 480453 的结构方程式

PROCEDURE

实验过程

A mixture of 6-bromo-2-hydroxy-N-methyl-1-naphthamide (2.50 g), tert-butyldimethylsilyl chloride (1.61 g), and imidazole (912 mg) in DMP (30 mL) was stirred for 2 h at room temperature. After dilution with water, the resulting mixture was extracted with AcOEt. The organic layer was washed with water and brine followed by concentrating in vacuo. The residue was passed through silica gel plug (hexane:AcOEt=1:1). The elute was concentrated, and the residue was washed with hexane to give the titled compound (3.33 g) as colorless needles.

WORKUP

后处理

  1. extractionAfter dilution with water, the resulting mixture was extracted with AcOEt
  2. washThe organic layer was washed with water and brine
  3. concentrationby concentrating in vacuo
  4. concentrationThe elute was concentrated
  5. washthe residue was washed with hexane