Nitromethane → HCID 22236902、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]([CH3:14])=[CH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].[N+:15]([CH3:18])([O-:17])=[O:16].C1CCN2C(=NCCC2)CC1>C(#N)C>[CH3:14][C:7]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1)([CH2:18][N+:15]([O-:17])=[O:16])[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]参加物
5
実験手順
A solution of 6 g of the compound obtained in Step 1, 3.36 ml of nitromethane and 4.26 ml of DBU dissolved in 120 ml of acetonitrile was heated to reflux for 36 hours. After the reaction was completed, the reaction solution was distilled under reduced pressure. The residue thus obtained was purified by a silica gel column chromatography using a mixture of ethyl acetate and n-hexane of 1:9 to obtain 1.8 g of the title compound as a syrup.
後処理
- temperaturewas heated
- temperatureto reflux for 36 hours
- distillationthe reaction solution was distilled under reduced pressure
- customThe residue thus obtained
- customwas purified by a silica gel column chromatography
- additiona mixture of ethyl acetate and n-hexane of 1:9
出典と根拠
- ORDレコード
- ord-995470827d67461cbbf0be5af4c91273
- 出典データセット
- uspto-grants-2006_03
- 特許番号
- US07012144B2
反応ノート
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