Sodium Sulfate → 3,5-Dimethyl-4-(hydroxymethyl)isoxazole

HRID 359822

반응식

HRID 359822 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([C:12]1[C:13]([CH3:18])=[N:14][O:15][C:16]=1[CH3:17])(OCC)=[O:8].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH3:18][C:13]1[C:12]([CH2:7][OH:8])=[C:16]([CH3:17])[O:15][N:14]=1

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 736348Ethyl 3,5-dimethylisoxazole-4-carboxylateHCID 21226445Aluminium lithium hydride2회

생성물 1

HCID 2895753,5-Dimethyl-4-(hydroxymethyl)isoxazole수율 75.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension of 23.53 g of lithium aluminum hydride in 600 ml of ether was added dropwise 64 g of 4-carbethoxy-3,5-dimethylisoxazole in 100 ml of ether at a rate so that gentle reflux occurred. The addition was complete in about two hours, and the mixture was stirred overnight under nitrogen. A saturated solution of sodium sulfate was added dropwise under nitrogen until the excess lithium aluminum hydride was decomposed. The resulting suspension was filtered and the filtrate concentrated to an oil which was distilled to give 36.4 g of 3,5-dimethyl-4-hydroxymethylisoxazole, b.p. 130°-140° C. (0.1 mm).

후처리

  1. temperaturethat gentle reflux
  2. additionThe addition
  3. filtrationThe resulting suspension was filtered
  4. concentrationthe filtrate concentrated to an oil which
  5. distillationwas distilled

출처 및 근거

ORD 기록
ord-216dd9ccd641402aab34f64cd3767c27
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05002960

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