Water → HCID 86678767、化合物
反応式
[CH3:1][C:2]([OH:8])([CH3:7])[C:3]#[C:4][CH2:5][OH:6].C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18].O>C1COCC1>[CH3:16][S:17]([O:6][CH2:5][C:4]#[C:3][C:2]([OH:8])([CH3:7])[CH3:1])(=[O:19])=[O:18]参加物
6
実験手順
To a solution of 4-methylpent-2-yne-1,4-diol (Synthesis 2001. 1013.) (1.00 g) in THF (40 mL) were added triethylamine (1.85 mL) and methanesulfonyl chloride (0.69 mL). The reaction mixture was stirred at room temperature overnight under a nitrogen atmosphere, water was added, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.57 g).
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-8b073f0c07e84f2d9b559d0dc971a751
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772277B2
反応ノート
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