Dichloromethane → HCID 68670764、化合物
反応式
O[CH2:2][C:3]1[CH:4]=[C:5]([C:11](O)([CH3:13])[CH3:12])[C:6]([CH3:10])=[N:7][C:8]=1[CH3:9].C(Cl)[Cl:16]>>[Cl:16][CH2:2][C:3]1[C:8]([CH3:9])=[N:7][C:6]([CH3:10])=[C:5]([C:11]([CH3:13])=[CH2:12])[CH:4]=1参加物
3
実験手順
To a stirring solution of 2-(5-(hydroxymethyl)-2,6-dimethylpyridin-3-yl)propan-2-ol in 10 mL of CH2Cl2 was added 1.5 mL of SO2Cl2. After 11 h at r.t., the solution was concentrated and CH2Cl2 and 10 mL of sat. NaHCO3 solution were added, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (20% Et2O/hexanes) provided 96.5 mg of the desired 3-(chloromethyl)-2,6-dimethyl-5-(prop-1-en-2-yl)pyridine as a mixture.
後処理
- concentrationthe solution was concentrated
- additionCH2Cl2 and 10 mL of sat. NaHCO3 solution were added
- customthe layers were separated
- washThe organic layer was washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customPurification by flash silica gel chromatography (20% Et2O/hexanes)
出典と根拠
- ORDレコード
- ord-74c2ebecbf054444940569c65eedfc13
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08299267B2
反応ノート
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