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Triethylamine → HCID 9848238、化合物

HRID 1455514
ノート
印刷プレビュー

反応式

HRID 1455514 の反応式
CN(C(ON1[N:17]=[N:16][C:15]2[C:10]1=[CH:11][CH:12]=[CH:13][CH:14]=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:25][CH:26]([N:28]1[CH2:33][CH2:32][N:31]([CH2:34][C:35]2[C:36]([C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)=[N:37][C:38]3[C:43]([C:44]=2[C:45](O)=[O:46])=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH2:30][CH2:29]1)[CH3:27].NN1CCCCCC1.CCN(CC)CC>C1COCC1.C(Cl)Cl>[N:16]1([NH:17][C:45]([C:44]2[C:43]3[C:38](=[CH:39][CH:40]=[CH:41][CH:42]=3)[N:37]=[C:36]([C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)[C:35]=2[CH2:34][N:31]2[CH2:32][CH2:33][N:28]([CH:26]([CH3:25])[CH3:27])[CH2:29][CH2:30]2)=[O:46])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 221981-AminohomopiperidineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 11280720HCID 11280720、化合物

生成物 1

HCID 9848238HCID 9848238、化合物

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

O-Benzotriazole-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HBTU) (156 mg, 0.41 mmol) was added to a stirred mixture of 3-(4-(1-methylethyl)-piperazin-1-ylmethyl)-2-phenyl-quinoline-4-carboxylic acid (100 mg, 0.26 mmol) [J. Med. Chem. 2001, 44, 1675-1689], 1-aminohomopiperidine (47 μL, 0.41 mmol) and Et3N (178 μL, 1.3 mmol) in THF (5 mL) and CH2Cl2 (1.5 mL), and the mixture was heated at reflux for 18 h under N2. The solvent was evaporated under reduced pressure, and the residue was dissolved in CH2Cl2 and washed with H2O, 0.5 N NaOH solution, and H2O. The organic phase was dried (MgSO4) and concentrated under reduced pressure. The residue was purified by reverse phase preparative HPLC affording, after basic work up, the desired hydrazide (28 mg, 17%). 1H NMR (CD3OD, 360 MHz), Major rotamer δ 8.05 (1H, d, J=8.3 Hz), 7.96 (1H, d, J=8.3 Hz), 7.83-7.75 (1H, m), 7.72-7.60 (1H, m), 7.55-7.43 (5H, m), 3.66 (2H, s), 3.24-3.17 (4H, m), 2.53 (1H, septet, J=6.5 Hz), 2.45-2.10 (8H, m), 1.86-1.72 (8H, m), 1.00 (6H, d, J=6.5 Hz). MS (ES+) C30H39N5O requires: 485, found: 486 (M+H+, 100%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 18 h under N2
  3. customThe solvent was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in CH2Cl2
  5. washwashed with H2O, 0.5 N NaOH solution, and H2O
  6. dry with materialThe organic phase was dried (MgSO4)
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by reverse phase preparative HPLC
  9. customaffording

出典と根拠

ORDレコード
ord-9f4cbe73575e46e998de0dbcab668905
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482457B2

反応ノート

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