Acetamide → 4-(4-Bromophenyl)-2-methyl-1,3-oxazole
反応式
[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6](=O)[CH2:7]Br)=[CH:4][CH:3]=1.[C:12]([NH2:15])(=[O:14])[CH3:13]>>[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]2[N:15]=[C:12]([CH3:13])[O:14][CH:7]=2)=[CH:4][CH:3]=1参加物
3
実験手順
4-Bromophenacyl bromide (21.3 g) and acetamide (11.3 g) were heated together at 130° C. under argon. After 2.5 h the reaction mixture was allowed to cool, and partitioned between water (150 ml) and Et2O (150 ml). The organic phase was washed with aqueous NaOH (0.5N), aqueous HCl (0.5M) and saturated aqueous NaCl solution (100 ml of each), dried (MgSO4) and evaporated to give a brown solid which was recrystallised from hexanes to give the title compound (D14) as an orange solid (4.1 g). LCMS electrospray (+ve) 239 (MH+).
後処理
- temperatureto cool
- custompartitioned between water (150 ml) and Et2O (150 ml)
- washThe organic phase was washed with aqueous NaOH (0.5N), aqueous HCl (0.5M) and saturated aqueous NaCl solution (100 ml of each),
- dry with materialdried (MgSO4)
- customevaporated
- customto give a brown solid which
- customwas recrystallised from hexanes
出典と根拠
- ORDレコード
- ord-ca041f5bd11a422190a1eca628cc90df
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08492375B2
反応ノート
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