Dimethylformamide → HCID 67244819、化合物
反応式
IC.CN([CH:6]=[O:7])C.[Br:8][C:9]1[CH:10]=[C:11]([CH2:14]O)[O:12][CH:13]=1.[H-].[Na+]>O.C(OCC)(=O)C>[Br:8][C:9]1[CH:10]=[C:11]([CH2:14][O:7][CH3:6])[O:12][CH:13]=1参加物
7
実験手順
Iodomethane (1.6 mL) was added to a DMF (15 mL) solution of (4-bromofuran-2-yl)methanol (3.0 g) as obtained in Example 18-(1). Under ice cooling, 60% sodium hydride (0.82 g) was added in divided portions, and the mixture was stirred for 1 hour and 40 minutes at room temperature. Ethyl acetate and water were added, and the organic layer was isolated. The extract was washed with water and brine sequentially, and dried over anhydrous magnesium sulfate. Then, the desiccant was filtered out, and the solvent was distilled off under reduced pressure to obtain partially purified 4-bromo-2-(methoxymethyl)furan (yellow oil) (3.9 g).
後処理
- customas obtained in Example 18-(1)
- customthe organic layer was isolated
- washThe extract was washed with water and brine sequentially
- dry with materialdried over anhydrous magnesium sulfate
- filtrationThen, the desiccant was filtered out
- distillationthe solvent was distilled off under reduced pressure
出典と根拠
- ORDレコード
- ord-9d2f670a34704710a4ac0d3cfa36bbdc
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073821B2
反応ノート
読み込み中…