1,3-Dichloroacetone → 4-Chloromethyl-2-propyloxazole

HRID 4398

반응식

HRID 4398 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]=1

참가 물질

5

반응물 3

HCID 107931,3-DichloroacetoneHCID 10927ButyramideHCID 516892Sodium Bicarbonate

생성물 1

HCID 201524274-Chloromethyl-2-propyloxazole

시약·촉매·용매 1

HCID 962Water용매

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

  1. temperatureAfter cooling
  2. extractionextracted with ethyl ether
  3. washThe extract was washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. 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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