Formamide → HCID 15005406、化合物
反応式
[CH:1]([NH2:3])=[O:2].Br[CH:5]([C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1)[C:6](=O)[CH3:7].C(=O)(O)[O-].[Na+]>ClCCl>[C:13]([C:12]1[CH:15]=[CH:16][C:9]([C:5]2[O:2][CH:1]=[N:3][C:6]=2[CH3:7])=[CH:10][CH:11]=1)#[N:14]参加物
5
実験手順
A stirred, two-phase mixture of formamide (0.6 ml, 15 mmol) and 4-(1-bromo-2-oxopropyl)benzonitrile (0.8 g, 3.4 mmol) was heated to 120° for 2 hours. After cooling, dichloromethane (15 ml) and saturated aqueous sodium bicarbonate (10 ml) were added, the organic phase was separated, dried (magnesium sulphate) and the solvent removed under reduced pressure to yield 0.4 g of an amorphous yellow solid. The product was purified by silica gel chromatography, eluting with dichloromethane to yield the title compound (0.29 g, 47%) as a pale yellow solid, m.p. 120°-121° C.
後処理
- temperaturewas heated to 120° for 2 hours
- temperatureAfter cooling
- customthe organic phase was separated
- dry with materialdried (magnesium sulphate)
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-4a776624bb534c6b85e61935c25d9dfc
- 出典データセット
- uspto-grants-1990_06
- 特許番号
- US04935430
反応ノート
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