Formic Acid → 11-Oxo-6,11-dihydrodibenzo[b,e]oxepine-2-carbaldehyde
反応式
[C:1]([C:3]1[CH:18]=[CH:17][C:6]2[O:7][CH2:8][C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11](=[O:12])[C:5]=2[CH:4]=1)#N.C(O)=[O:20]>[Ni]>[O:12]=[C:11]1[C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=2[CH2:8][O:7][C:6]2[CH:17]=[CH:18][C:3]([CH:1]=[O:20])=[CH:4][C:5]1=2参加物
4
実験手順
Heat a mixture of 5.0 gm. of 2-cyano-6.11-dihydro-11-oxodibenz[b,e]oxepin and 4.0 gm. of Raney nickel alloy in 60 ml. of 75% (v/v) aqueous formic acid at reflux for 1.5 hours. Cool to room temperature and filter. Concentrate to small volume and extract with methylene chloride. Wash the extract with water and with 1 N sodium bicarbonate until neutral. Dry the neutral extract over sodium sulfate and concentrate to dryness to obtain the title product.
後処理
- temperatureHeat
- additiona mixture of 5.0 gm
- filtrationfilter
- concentrationConcentrate to small volume
- extractionextract with methylene chloride
- washWash the
- extractionextract with water and with 1 N sodium bicarbonate until neutral
- customDry the
- extractionneutral extract over sodium sulfate
- concentrationconcentrate to dryness
出典と根拠
- ORDレコード
- ord-2a8e7d02ece34d5786073bf50b2ddd3f
- 出典データセット
- uspto-grants-1981_08
- 特許番号
- US04282365
反応ノート
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