반응 #6460

반응 방정식

5-benzoyl-3,4-dihydro-2H-1,4-benzoxazine

pyridine

bromoacetyl bromide

water

→

4-bromoacetyl-5-benzoyl-3,4-dihydro-2H-1,4-benzoxazine

수율 69.4%

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타The organic layer was separated
3. 3
   세척washed with water
4. 4
   건조dried over magnesium sulfate
5. 5
   기타evaporated
6. 6
   기타The residue was crystallized with a mixture of diisopropyl ether and ethyl acetate
7. 7
   여과The crystals were collected by filtration

실험 절차

To a solution of 5-benzoyl-3,4-dihydro-2H-1,4-benzoxazine (5.74 g), pyridine (1.9 g) and methylene chloride (100 ml) was dropwise added a solution of bromoacetyl bromide (5.82 g) in methylene chloride (5 ml) at room temperature. After the mixture was stirred for 1.0 hour at the same temperature, water (100 ml) was added thereto under stirring. The organic layer was separated, washed with water, dried over magnesium sulfate and evaporated. The residue was crystallized with a mixture of diisopropyl ether and ethyl acetate. The crystals were collected by filtration to give 4-bromoacetyl-5-benzoyl-3,4-dihydro-2H-1,4-benzoxazine (6.0 g).

출처