Ethyl pyruvate → Ethyl 2-hydroxyiminopropionate
反応式
[C:1]([O:6][CH2:7][CH3:8])(=[O:5])[C:2]([CH3:4])=O.Cl.[NH2:10][OH:11].C([O-])(=O)C.[Na+]>C(O)C>[OH:11]/[N:10]=[C:2](\[CH3:4])/[C:1]([O:6][CH2:7][CH3:8])=[O:5]参加物
5
実験手順
A mixture of ethyl pyruvate (9.50 g), hydroxylamine hydrochloride (6.82 g), sodium acetate (10.1 g) and ethanol (150 ml) was heated under reflux for 17 hours. The reaction mixture was concentrated, and the residue was diluted with water and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and then concentrated. The residual crystals were recrystallized from ethyl acetate-hexane to obtain ethyl E-2-hydroxyiminopropionate (6.33 g, yield 59%) as colorless crystals. m.p. 98-99° C.
後処理
- temperaturewas heated
- temperatureunder reflux for 17 hours
- concentrationThe reaction mixture was concentrated
- additionthe residue was diluted with water
- extractionextracted with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe residual crystals were recrystallized from ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-6135cca9cf6545ef8e843fdab3262949
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06924300B2
反応ノート
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