1,3-Dichloroacetone → 4-Chloromethyl-2-propyloxazole
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 130 °C
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-7d658abe348645fab4f8f7ddde1e6c72
- 출처 데이터셋
- uspto-grants-1988_02
- 특허 번호
- US04725610
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