Isopropanol → 77092-47-8
反応式
[H-].[Na+].[CH:3]([OH:6])([CH3:5])[CH3:4].Br[CH2:8][CH:9]([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12]>C(Cl)Cl>[CH2:11]([O:10][CH:9]([O:13][CH2:14][CH3:15])[CH2:8][O:6][CH:3]([CH3:5])[CH3:4])[CH3:12]参加物
5
実験手順
NaH (3.35 g, 84 mmol) was added to isopropanol (5.38 mL, 69.9 mmol) at 0° C. The reaction mixture was stirred at room temperature for 30 min followed by the addition of 2-bromo-1,1-diethoxyethane (7.89 mL, 52.4 mmol). The tube was sealed, heated to 120° C. and stirred overnight. The sealed tube was cooled to room temperature and the contents were dissolved in DCM and washed with water twice. The organic layer was separated, dried over sodium sulfate and concentrated in vacuo to give 2-(2,2-diethoxy-ethoxy)-propane, which was hydrolyzed according to the method described in example 29 to give crude isopropoxy-acetaldehyde.
後処理
- customThe tube was sealed
- temperatureheated to 120° C.
- stirringstirred overnight
- temperatureThe sealed tube was cooled to room temperature
- washwashed with water twice
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-a4b473e1800146bcbd7c953911ff36d5
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08519134B2
反応ノート
読み込み中…