Propanal → 4-Nitro-3-hexanol
反応式
[N+:1](CCC)([O-:3])=[O:2].[CH2:7]1[CH2:17][CH2:16]N2[C:10](=NCCC2)[CH2:9][CH2:8]1.C(=[O:21])CC>C(OCC)(=O)C>[OH:21][CH:7]([CH2:17][CH3:16])[CH:8]([N+:1]([O-:3])=[O:2])[CH2:9][CH3:10]参加物
5
実験手順
A reaction vessel was replaced with nitrogen, and 1-nitropropane (8.93 ml, 100 mmol) and dry-THF (50 ml) were added. After DBU (1,8-diazabicyclo[5.4.0]-7-undecene) (1.5 ml, 10 mmol) had been added, propionaldehyde (4.68 ml, 100 mmol) was added while the vessel was cooled in an ice bath. After the mixture had been stirred at room temperature for 10 hours, ethyl acetate (100 ml) was added, and the whole was washed with dilute hydrochloric acid, water, and a saturated salt solution. The organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure to yield 4-hydroxy-3-nitrohexane (12.33 g, 84% yield).
後処理
- dry with materialdry-THF (50 ml)
- additionwere added
- temperaturewas cooled in an ice bath
- washthe whole was washed with dilute hydrochloric acid, water
- dry with materialThe organic layer was dried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-d86b3209a13340678209556d5317e7fd
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08021915B2
反応ノート
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