反応式
C[Si]([N:5]=[C:6]=[O:7])(C)C.CO[C:10]([CH:12]([NH:16][CH:17]1[CH2:22][CH2:21][N:20]([C:23]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:24])[CH2:19][CH2:18]1)[CH2:13][CH:14]=[CH2:15])=[O:11]>CN(C1C=CN=CC=1)C.C1COCC1>[CH2:13]([CH:12]1[N:16]([CH:17]2[CH2:18][CH2:19][N:20]([C:23]([O:25][CH2:26][C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])[CH2:21][CH2:22]2)[C:6](=[O:7])[NH:5][C:10]1=[O:11])[CH:14]=[CH2:15]参加物
5
反応条件
- 温度
- 50 °C
実験手順
Trimethylsilyl isocyanate (1.66 g, 14.4 mmol) was added to a solution of benzyl 4-{[1-(methoxycarbonyl)but-3-en-1-yl]amino}piperidine-1-carboxylate (2.00 g, 5.77 mmol) and DMAP (71 mg, 0.57 mmol) in THF (30 mL) at room temperature. The reaction was heated at 50° C. for 48 h. The reaction was quenched with saturated aqueous sodium bicarbonate, extracted with methylene chloride (3×), dried over sodium sulfate, filtered and evaporated to give the crude product. The crude product was purified by chromatography (silica gel, 0 to 20% methanol in methylene chloride gradient elution), which gave the title compound (1.66 g). MS 358.2 (M+1).
後処理
- customThe reaction was quenched with saturated aqueous sodium bicarbonate
- extractionextracted with methylene chloride (3×)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- customto give the crude product
- customThe crude product was purified by chromatography (silica gel, 0 to 20% methanol in methylene chloride gradient elution), which
出典と根拠
- ORDレコード
- ord-5d63dab5c7f94db1a5c18b0230d314ab
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07772224B2
関連ノート
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