反応式
[O:1]=[C:2]([CH3:11])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]([OH:10])=O.C(N(CC)CC)C.C(Cl)CCl.[NH2:23][C@@H:24]([CH2:33][N:34]1[CH2:39][CH2:38][O:37][CH2:36][CH2:35]1)[C@H:25]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[OH:26]>C(Cl)Cl.CO>[O:1]=[C:2]([CH3:11])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]([NH:23][C@@H:24]([CH2:33][N:34]1[CH2:35][CH2:36][O:37][CH2:38][CH2:39]1)[C@H:25]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[OH:26])=[O:10]参加物
実験手順
A mixed solvent of methylene chloride:methanol=9:1 (20 ml), 7-oxooctanoic acid (700 mg, 4.4 mmol), triethylamine (1.40 ml, 10.0 mmol) and EDC (1.15 g, 6.0 mmol) were added to (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol (944.0 mg, 4.0 mmol), followed by stirring overnight. Methylene chloride (100 ml) was added to the reaction solution. After washed with a saturated sodium hydrogen carbonate solution (50 ml), water (50 ml) and saturated brine (50 ml) successively, the organic layer was dried over sodium sulfate and filtered, and the solvent was evaporated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (chloroform:ethanol=20:1) to obtain the title compound (890 mg, yield 59%) as colorless oil.
後処理
- washAfter washed with a saturated sodium hydrogen carbonate solution (50 ml), water (50 ml) and saturated brine (50 ml) successively
- dry with materialthe organic layer was dried over sodium sulfate
- filtrationfiltered
- customthe solvent was evaporated under reduced pressure
- customThe resulting crude product was purified by silica gel column chromatography (chloroform:ethanol=20:1)
出典と根拠
- ORDレコード
- ord-46f28482c5de43128f1566b914bbe8e9
- 出典データセット
- uspto-grants-2002_06
- 特許番号
- US06407064B2
関連ノート
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