Triethylamine → HCID 21083245, 화합물

HRID 347633노트

반응식

HRID 347633 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21083245HCID 21083245, 화합물

시약·촉매·용매 1

HCID 142844-(Dimethylamino)pyridine촉매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-299cf132274b4f57a0d398e708e6d702
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176195B2

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