Реакция #1049

Уравнение реакции

methylene chloride

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

ammonium chloride

bromoacetyl bromide

→

compound ( 8 )

Выход 65.0%

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

Выход 65.0%

Растворители

triethylamine

Условия реакции

Обработка

1. 1
   Экстракцияextraction
2. 2
   ПромывкаThe extract was washed with saturated saline
3. 3
   Другоеdried
4. 4
   Фильтрацияfiltered
5. 5
   Концентрированиеconcentrated under reduced pressure
6. 6
   Другоеto obtain a residue which
7. 7
   Другоеwas then purified by silica gel column chromatography (methylene chloride:methanol=25:1)

Методика

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%).

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