Methanol → HCID 53798545、化合物
反応式
[CH3:1][C:2](=[CH:4][CH2:5][C:6](=[N:9][OH:10])[CH2:7][CH3:8])[CH3:3].CO.C[O-].[Na+].O1C[CH2:19][CH2:18][CH2:17]1.C(Br)C=C>>[CH3:1][C:2](=[CH:4][CH2:5][C:6](=[N:9][O:10][CH2:19][CH:18]=[CH2:17])[CH2:7][CH3:8])[CH3:3]参加物
反応条件
- 温度
- 0 °C
実験手順
A reactor was charged with 1 mole of 2-methyl-5-hydroxyimino-2-heptene, 8 moles of methanol containing 1.2 moles of sodium methylate, and 10 moles of tetrahydrofuran (THF). The mixture was cooled to 0° C., and with stirring, 1.3 moles of allyl bromide was added dropwise over 5 minutes. The mixture was stirred at room temperature for one day. The reaction mixture was concentrated, and 40 parts of methylene chloride was added. The mixture was washed with water, and the solvent was evaporated. The residue was purified by silica gel column chromatography to give 2-methyl-5-allyloxyimino-2-heptene in a yield of 80 mole %. Identification of this compound was performed by using IR, NMR and mass spectra (the same techniques were used to identify compounds appearing hereinafter).
後処理
- stirringThe mixture was stirred at room temperature for one day
- concentrationThe reaction mixture was concentrated
- addition40 parts of methylene chloride was added
- washThe mixture was washed with water
- customthe solvent was evaporated
- customThe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-7475892712fd458aa88cf7d94d0c1dda
- 出典データセット
- uspto-grants-1990_03
- 特許番号
- US04906768
反応ノート
読み込み中…