Hydrochloric Acid → [3-Methyl-4-(methylthio)phenyl]methanol
反応式
[BH4-].[Na+].[CH3:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[S:12][CH3:13])[CH:7]=[O:8].Cl>C(O)C>[CH3:3][C:4]1[CH:5]=[C:6]([CH2:7][OH:8])[CH:9]=[CH:10][C:11]=1[S:12][CH3:13]参加物
5
実験手順
Sodium borohydride (1.40 g, 0.037 mol) was added to an ice-bath cooled solution of the product of example 28 step a) (6.16 g, 0.037 mol) in ethanol (50 ml). After 1 hour, the reaction mixture was neutralised by careful addition of aqueous hydrochloric acid (2 molar) and concentrated in vacuo to remove the organic solvent. The remaining aqueous solution was then extracted with ethyl acetate (×3). The combined organic layers were dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to yield the sub-title compound as a brown oil (6 g) in quantitative yield.
後処理
- concentrationconcentrated in vacuo
- customto remove the organic solvent
- extractionThe remaining aqueous solution was then extracted with ethyl acetate (×3)
- dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-7109ee3449164ef6b5f238553cf7f8f9
- 出典データセット
- uspto-grants-2004_09
- 特許番号
- US06790850B1
反応ノート
読み込み中…