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

HRID 394115ノート

反応式

HRID 394115 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]([CH:18]=[C:19]2[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:21][CH2:20]2)[CH:15]=[C:14]2[C:9]=1[CH2:10][NH:11][C:12](=[O:40])[N:13]2[C:32]1[C:37]([Cl:38])=[CH:36][CH:35]=[CH:34][C:33]=1[Cl:39]>C(OCC)(=O)C.O.[Pt](=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][CH:19]2[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:30])([CH3:31])[CH3:29])=[O:26])[CH2:21][CH2:20]2)[CH:15]=[C:14]2[C:9]=1[CH2:10][NH:11][C:12](=[O:40])[N:13]2[C:32]1[C:33]([Cl:39])=[CH:34][CH:35]=[CH:36][C:37]=1[Cl:38]

参加物

4

反応物 1

HCID 22648188Tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methylene}piperidine-1-carboxylate

生成物 1

HCID 22647967Tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 11139377Platinum dioxide monohydrate触媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methylene}piperidine-1-carboxylate (EXAMPLE AAA18, STEP C, 150 mg, 0.25 mmol) in ethyl acetate (4 mL) was purged and filled with nitrogen. To this was added platinum (IV) oxide hydrate (30 mg, 20% weight). The mixture was evacuated and filled with hydrogen via balloon. Then the reaction was stirred at rt under hydrogen for 1 h, filtered through celite and rinsed with ethyl acetate and methanol. Removal of the solvent provided tert-butyl 4-{[5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-2-oxo-1,2,3,4-tetrahydroquinazolin-7-yl]methyl}piperidine-1-carboxylate as a white solid used directly for the next step.

後処理

  1. additionfilled with nitrogen
  2. customThe mixture was evacuated
  3. additionfilled with hydrogen via balloon
  4. filtrationfiltered through celite
  5. washrinsed with ethyl acetate and methanol
  6. customRemoval of the solvent

出典と根拠

ORDレコード
ord-7336037e33ca451ba379123915055fd9
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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