反応式
CN1CCOCC1.C(OC(Cl)=O)C(C)C.[CH3:16][CH2:17][CH2:18][CH2:19][C:20]1[CH:21]=[CH:22][C:23]([C:26]([OH:28])=O)=[N:24][CH:25]=1.Cl.[CH3:30][O:31][NH:32][CH3:33]>C(Cl)Cl>[CH3:30][O:31][N:32]([CH3:33])[C:26]([C:23]1[CH:22]=[CH:21][C:20]([CH2:19][CH2:18][CH2:17][CH3:16])=[CH:25][N:24]=1)=[O:28]参加物
6
実験手順
Add N-methylmorpholine (1.22 mL, 11.1 mmol) and isobutylchloroformate (1.44 mL, 11.1 mmol) to a solution of fusaric acid (2.0 g, 11.1 mmol) in methylene chloride at 0° C. After 15 minutes add O,N-dimethylhydroxylamine hydrochloride (1.1 g, 11.1 mmol) and N-methylmorpholine (1.22 mL, 11.1 mmol). Stir the reaction for at 0° C. 15 minutes and then room temperature for 19 hours. Dilute the reaction with methylene chloride and wash with water (1×50 mL), 10% aqueous citric acid (1×50 mL), brine (1×50 mL), saturated aqueous sodium bicarbonate (1×50 mL), and brine (1×50 mL). Dry the organic solution with sodium sulfate, filter, and concentrate in vacuo to provide the title compound 3.2 g (100%) as a clear yellow oil.
後処理
- customthe reaction for at 0° C
- additionDilute
- washwash with water (1×50 mL), 10% aqueous citric acid (1×50 mL), brine (1×50 mL), saturated aqueous sodium bicarbonate (1×50 mL), and brine (1×50 mL)
- dry with materialDry the organic solution with sodium sulfate
- filtrationfilter
- concentrationconcentrate in vacuo
出典と根拠
- ORDレコード
- ord-65b54fd4021c4f05b80f48b57b7904b7
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07365066B2
関連ノート
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