HCID 178482482、化合物 → HCID 178482481、化合物

HRID 1509086ノート

反応式

HRID 1509086 の反応式
C(OC(=O)[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:27]([C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[CH:26][C:25]4[C:24]5=[N:34][NH:35][C:36]([NH:37][CH3:38])=[C:23]5[CH2:22][CH2:21][C:20]=4[N:19]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)(C)(C)C>C(O)(C(F)(F)F)=O>[NH2:7][C:8]1([C:12]2[CH:13]=[CH:14][C:15]([C:18]3[C:27]([C:28]4[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=4)=[CH:26][C:25]4[C:24]5=[N:34][NH:35][C:36]([NH:37][CH3:38])=[C:23]5[CH2:22][CH2:21][C:20]=4[N:19]=3)=[CH:16][CH:17]=2)[CH2:11][CH2:10][CH2:9]1

参加物

3

反応物 1

HCID 178482482HCID 178482482、化合物

生成物 1

HCID 178482481HCID 178482481、化合物収率 81.7%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

tert-butyl(1-(4-(3-(methylamino)-8-phenyl-4,5-dihydro-2H-pyrazolo[3,4-f]quinolin-7-yl)phenyl)cyclobutyl)carbamate (47 mg, 0.090 mmol) was dissolved in TFA (2 mL) and stirred for 30 seconds. The solution was immediately concentrated to dryness under reduced pressure. The residue was dissolved in diethyl ether (˜2 mL) and concentrated to dryness under reduced pressure three times. The residue was then slurried in diethyl ether (2 mL) and after settling the supernatant solvent removed by pipette. This was repeated three times. The remaining solvent was removed under reduced pressure and freeze-dried to give the desired product as an off-white solid (31 mg, 53% yield). 1H-NMR (500 MHz, CD3OD) δ 8.08 (1H, s), 7.50 (2H, d), 7.44 (2H, d), 7.30-7.50 (3H, m), 7.23-7.27 (2H, m), 3.30 (2H, t), 2.98 (3H, s), 2.87 (2H, t), 2.73-2.81 (2H, m), 2.54-2.64 (2H, m), 2.19-2.31 (1H, m), 1.92-2.04 (1H, m). LCMS (Method A) RT=3.28 min, M+H+=422.18.

後処理

  1. concentrationThe solution was immediately concentrated to dryness under reduced pressure
  2. dissolutionThe residue was dissolved in diethyl ether (˜2 mL)
  3. concentrationconcentrated to dryness under reduced pressure three times
  4. customremoved by pipette
  5. customThe remaining solvent was removed under reduced pressure
  6. customfreeze-dried

出典と根拠

ORDレコード
ord-b2a387b910fe43e0a11455ee1ba6d91a
出典データセット
uspto-grants-2015_12
特許番号
US09221838B2

反応ノート

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