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

HRID 967

反応式

HRID 967 の反応式
C(#N)C.Br[CH2:5][C:6]([NH:8][CH:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[O:13][CH2:12][CH2:11][CH2:10]1)=[O:7].[O:20]([C:27]1[CH:32]=[CH:31][C:30]([CH:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(N(CC)CC)C>[O:20]([C:27]1[CH:32]=[CH:31][C:30]([CH:33]2[CH2:38][CH2:37][N:36]([CH2:5][C:6]([NH:8][CH:9]3[C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=4[O:13][CH2:12][CH2:11][CH2:10]3)=[O:7])[CH2:35][CH2:34]2)=[CH:29][CH:28]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 110759844-(4-Phenoxyphenyl)piperidineHCID 196942705-(2-Bromoacetylamino)-2,3,4,5-tetrahydro-1-benzoxepine

生成物 1

HCID 196942535-[2-(4-(4-Phenoxyphenyl)piperidin-1-yl)acetylamino]-2,3,4,5-tetrahydro-1-benzoxepine収率 98%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

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%).

後処理

  1. temperatureThis was heated
  2. temperatureat reflux for 3 hours
  3. extractionextraction
  4. customThe extract was dried
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto obtain a residue which
  8. customwas then purified by silica gel column chromatography (methylene chloride:methanol=25:1)

出典と根拠

ORDレコード
ord-23b3904cefa54993927e4b9f165740eb
出典データセット
uspto-grants-1998_03
特許番号
US05723475

関連ノート

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