반응 #1049

반응 방정식

methylene chloride

5-amino-2,3,4,5-tetrahydro-1-benzoxepine

ammonium chloride

bromoacetyl bromide

→

compound ( 8 )

수율 65.0%

5-(2-bromoacetylamino)-2,3,4,5-tetrahydro-1-benzoxepine

수율 65.0%

용매

triethylamine

반응 조건

후처리

1. 1
   추출extraction
2. 2
   세척The extract was washed with saturated saline
3. 3
   기타dried
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure
6. 6
   기타to obtain a residue which
7. 7
   기타was then purified by silica gel column chromatography (methylene chloride:methanol=25:1)

실험 절차

To a 5 ml methylene chloride solution of 150 mg of 5-amino-2,3,4,5-tetrahydro-1-benzoxepine (Japanese Unexamined Patent Publication (Kokai) No. 4-178381) and 0.15 ml of triethylamine was added dropwise, under ice cooling, 0.08 ml of bromoacetyl bromide. This was then stirred at room temperature for 1 hour. To the reaction was added 5 ml of a saturated aqueous solution of ammonium chloride, then extraction was performed with methylene chloride. The extract was washed with saturated saline, dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol=25:1) to obtain the above-referenced compound (8) in an amount of 165 mg (yield of 65%).

출처