Water → Tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}piperazine-2-carboxylate

HRID 394105ノート

反応式

HRID 394105 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:17]=[C:16]([CH2:18][N:19]2[CH2:24][CH2:23][N:22](C(C)C)[CH:21]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:20]2)[CH:15]=[C:14]2[C:9]=1[CH2:10][NH:11][C:12](=[O:43])[N:13]2[C:35]1[C:40]([Cl:41])=[CH:39][CH:38]=[CH:37][C:36]=1[Cl:42].O>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:17]=[C:16]([CH2:18][N:19]2[CH2:24][CH2:23][NH:22][CH:21]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:20]2)[CH:15]=[C:14]2[C:9]=1[CH2:10][NH:11][C:12](=[O:43])[N:13]2[C:35]1[C:40]([Cl:41])=[CH:39][CH:38]=[CH:37][C:36]=1[Cl:42]

参加物

4

反応物 2

HCID 962WaterHCID 10233169Tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}-1-isopropylpiperazine-2-carboxylate

生成物 1

HCID 22648143Tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}piperazine-2-carboxylate

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To the solution of tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}-1-isopropylpiperazine-2-carboxylate (EXAMPLE AAA11, 30 mg, 0.047 mmol) in trifluoroacetic acid (0.6 mL) was added water (0.03 mL). The reaction was stirred at rt for 20 h. Removal of the solvent and subsequent addition of ether resulted in a white precipitate. Filtration of the precipitate followed by washing with ether provided the title compound. 1H NMR (CDCl3, 500 MHz): δ 1.22 (d, 3H, J=7.0 Hz), 1.24 (d, 3H, J=6.9 Hz), 3.12(m, 2H), 3.30 (m, 1H), 3.44 (m, 1H), 3.50 (abq, 2H, J=7.1 Hz), 3.74 (m, 1H), 3.81 (m, 1H), 3.96 (m, 1H), 4.07 (m, 1H), 4.28 (dd, 1H, J1=14.6 Hz, J2=5.7 Hz), 4.42 (dd, 1H, J1=14.9 Hz, J2=10.1 Hz), 5.80 (brs, 1H), 6.13 (d, 1H, J=9.8 Hz), 6.95 (s, 1H), 7.32-7.58 (m, 7H). MS (API-ES+): 589 (M+H).

後処理

  1. customRemoval of the solvent and subsequent addition of ether
  2. customresulted in a white precipitate
  3. filtrationFiltration of the precipitate
  4. washby washing with ether

出典と根拠

ORDレコード
ord-0507c88ec8c34b1c90373eb2b45b9290
出典データセット
uspto-grants-2004_10
特許番号
US06809199B2

反応ノート

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