1,3-Dichloroacetone → 4-Chloromethyl-2-propyloxazole
反応式
[C:1]([NH2:6])(=[O:5])[CH2:2][CH2:3][CH3:4].[Cl:7][CH2:8][C:9]([CH2:11]Cl)=O.C(=O)(O)[O-].[Na+]>O>[Cl:7][CH2:8][C:9]1[N:6]=[C:1]([CH2:2][CH2:3][CH3:4])[O:5][CH:11]=1参加物
5
反応条件
- 温度
- 130 °C
実験手順
A mixture of butyramide (19.88 g) and 1.3-dichloroacetone (24.14 g) was heated at 130° C. for 1.5 hours. After cooling, the mixture was diluted with water, neutralized with aqueous sodium bicarbonate solution and extracted with ethyl ether. The extract was washed with water, dried (MgSO4) and concentrated. The residue was purified by chromatography on silica gel with acetone-hexane (1:9) to yield 4-chloromethyl-2-propyloxazole as an oil (10.70 g 35.3%). NMR (CDCl3)δ: 0.97 (3H, t, J=7.5 Hz), 1.79 (2H, sext, J=7.5 Hz), 2.72 (2H, t, J=7.5 Hz), 4.47 (2H, s), 7.53 (1H, s).
後処理
- temperatureAfter cooling
- extractionextracted with ethyl ether
- washThe extract was washed with water
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe residue was purified by chromatography on silica gel with acetone-hexane (1:9)
出典と根拠
- ORDレコード
- ord-7d658abe348645fab4f8f7ddde1e6c72
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04725610
反応ノート
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