Sodium → HCID 22768158、化合物

HRID 1764403ノート

反応式

HRID 1764403 の反応式
[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]

参加物

5

反応物 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 13309592Carboxazole

生成物 1

HCID 22768158HCID 22768158、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b404bf6641774d6aa51d45455d4170ff
出典データセット
uspto-grants-1978_09
特許番号
US04116671

反応ノート

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