反応式
[C:1]([O:5][C:6]([N:8]([CH2:20][C:21]1[CH:36]=[CH:35][C:24]([C:25]([O:27]CC2C=CC=CC=2)=[O:26])=[CH:23][CH:22]=1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CCO>[C:1]([O:5][C:6]([N:8]([CH2:20][C:21]1[CH:22]=[CH:23][C:24]([C:25]([OH:27])=[O:26])=[CH:35][CH:36]=1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
実験手順
H2 (1 atm) was bubbled slowly trough a suspension of 10% Pd/C (917 mg) in EtOH (25 mL) for 15 min at rt. To this suspension was then added a solution of benzyl 4-({(tert-butoxycarbonyl)[4-(trifluoromethyl)benzyl]amino}methyl)benzoate (4.303 g, 8.61 mmol) diluted in EtOH (5 mL). The resulting reaction mixture was stirred under 1 atm H2 for 4.5 h at rt. The reaction mixture was filtered over a pad of celite to remove the catalyst. EtOH was evaporated to afford the title compound as a colorless oil used in the next steps without further purification (3.520 g, 99%). 1H NMR (CDCl3, 300 MHz) δ 8.11 (d, J=8.1 Hz, 2H), 7.62 (d, J=8.1 Hz, 2H), 7.45-7.21 (m, 4H), 5.54 (s, 2H), 4.45 (s, 2H), 1.50 (s, 9H). HPLC (Condition A), Rt: 5.42 min (HPLC purity: 96.1%).
後処理
- customH2 (1 atm) was bubbled slowly trough
- additiona suspension of 10% Pd/C (917 mg) in EtOH (25 mL) for 15 min at rt
- customThe resulting reaction mixture
- filtrationThe reaction mixture was filtered over a pad of celite
- customto remove the catalyst
- customEtOH was evaporated
出典と根拠
- ORDレコード
- ord-f816f36cffc843c6ae46541ae267e55c
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07592477B2
関連ノート
読み込み中…