HRID1444690

反应详情

EQUATION

反应方程式

HRID 1444690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of N-(2-bromophenethyl)-2,2,2-trifluoroacetamide (8.88 g, 30 mmol) and paraformaldehyde (13.5 g, 0.45 mol) in 45 mL of glacial acetic acid at room temperature was slowly added 30 mL of sulfuric acid (96.6%). After stirring at room temperature overnight, the reaction mixture was quenched with ice water and extracted with EtOAc, washed with brine and Sat. NaHCO3 and dried over Na2SO4. After concentration, flash chomatography (SiO2, hexane/DCM=1:1) gave of 1-(5-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-2,2,2-trifluoroethanone as a white solid.

WORKUP

后处理

  1. customthe reaction mixture was quenched with ice water
  2. extractionextracted with EtOAc
  3. washwashed with brine and Sat. NaHCO3
  4. dry with materialdried over Na2SO4
  5. concentrationAfter concentration, flash chomatography (SiO2, hexane/DCM=1:1)