反応 #1063

反応方程式

acetonitrile

compound ( 8 )

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

compound ( 4 )

4-(4-phenoxyphenyl)piperidine

→

compound ( 28 )

収率 98.0%

5-[2-(4-(4-phenoxyphenyl)piperidin-1-yl)acetylamino]-2,3,4,5-tetrahydro-1-benzoxepine

収率 98.0%

溶媒

triethylamine

反応条件

後処理

1. 1
   温度This was heated
2. 2
   温度at reflux for 3 hours
3. 3
   抽出extraction
4. 4
   その他The extract was dried
5. 5
   ろ過filtered
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他to obtain a residue which
8. 8
   その他was then purified by silica gel column chromatography (methylene chloride:methanol=25:1)

実験手順

To a 5 ml acetonitrile solution of 190 mg of the compound (8) synthesized in Reference Example 8 were added 184 mg of the compound (4) synthesized in Reference Example 4 and 0.14 ml of triethylamine. This was heated at reflux for 3 hours. To the reaction was added 10 ml of ice water, then extraction was performed with ethyl acetate. The extract was 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-identified compound (28) in an amount of 300 mg (yield of 98%).

出典