Sodium → HCID 22768158, 화합물

HRID 461352노트

반응식

HRID 461352 반응식
[CH3:1][O-].[Na+].[Na].[C:5]([C:9]1[O:13][N:12]=[C:11]([NH:14][C:15](=[O:18])[O:16][CH3:17])[CH:10]=1)([CH3:8])([CH3:7])[CH3:6]>CO>[CH3:1][N:14]([C:11]1[CH:10]=[C:9]([C:5]([CH3:8])([CH3:6])[CH3:7])[O:13][N:12]=1)[C:15](=[O:18])[O:16][CH3:17]

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 13309592Carboxazole

생성물 1

HCID 22768158HCID 22768158, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To the sodium methoxide obtained by mixing sodium (1.57 g) with anhydrous methanol (45 ml), methyl N-(5-t-butyl-3-isoxazolyl)carbamate (12.88 g) is added. The resultant mixture is stirred at room temperature for 10 minutes, and the methanol is evaporated under reduced pressure. The residue is mixed with anhydrous benzene (100 ml) and dimethyl sulfate (8.61 g). The resultant mixture is stirred for 1 hour and refluxed for 1 hour. After cooling, the precipitate is filtered off. The organic layer is washed with an aqueous saturated solution of sodium bicarbonate and water in order, dried over anhydrous sodium sulfate, and the solvent is evaporated. The residue is distilled to give methyl N-methyl-N-(5-t-butyl-3-isoxazolyl)carbamate (11.45 g) as a distillate boiling at 84.0° to 87.0° C/0.55 mm Hg.

후처리

  1. additionis added
  2. customthe methanol is evaporated under reduced pressure
  3. additionThe residue is mixed with anhydrous benzene (100 ml) and dimethyl sulfate (8.61 g)
  4. temperaturerefluxed for 1 hour
  5. temperatureAfter cooling
  6. filtrationthe precipitate is filtered off
  7. washThe organic layer is washed with an aqueous saturated solution of sodium bicarbonate and water in order
  8. dry with materialdried over anhydrous sodium sulfate
  9. customthe solvent is evaporated
  10. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-4c450a4305974a99b23f6a7e6c9fec02
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062861

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