Triethylamine → HCID 21083245、化合物

HRID 347633ノート

反応式

HRID 347633 の反応式
[NH:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][CH2:4][CH2:3][CH2:2]1.[C:12]([C:14]1[CH:22]=[CH:21][C:17]([C:18](O)=[O:19])=[CH:16][CH:15]=1)#[N:13].C(N(CC)CC)C>CN(C)C1C=CN=CC=1>[C:12]([C:14]1[CH:22]=[CH:21][C:17]([C:18]([N:1]2[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[CH2:5][CH2:4][CH2:3][CH2:2]2)=[O:19])=[CH:16][CH:15]=1)#[N:13]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 120874-Cyanobenzoic acidHCID 5765032,3,4,5-tetrahydro-1H-1-benzazepine

生成物 1

HCID 21083245HCID 21083245、化合物

試薬・触媒・溶媒 1

HCID 142844-(Dimethylamino)pyridine触媒

実験手順

To a solution of 2,3,4,5-tetrahydro-1H-1-benzazepine (1.05 g, 7.14 mmol) in dichloromethans (40 ml) were added 4-cyanobenzoic acid (1.26 g, 8.57 mmol), triethylamine (1.00 g, 7.14 mmol), 4-(dimethylamino)pyridine (0.87 g, 7.14 mmol) and WSCDI (2.86 g, 14.28 mmol). The mixture was stirred at reflux for 18 h, cooled and evaporated in vacuo. The residue was partitioned between EtOAc and 1M KHSO4. The organic layer was washed with saturated sodium bicarbonate solution and brine, dried over MgSO4, and concentrated in vacuo to give a white solid; yield 1.50 g (76%).

後処理

  1. temperatureat reflux for 18 h
  2. temperaturecooled
  3. customevaporated in vacuo
  4. customThe residue was partitioned between EtOAc and 1M KHSO4
  5. washThe organic layer was washed with saturated sodium bicarbonate solution and brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customto give a white solid

出典と根拠

ORDレコード
ord-299cf132274b4f57a0d398e708e6d702
出典データセット
uspto-grants-2007_02
特許番号
US07176195B2

反応ノート

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