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Water → HCID 44218625、化合物

HRID 474187
ノート
印刷プレビュー

反応式

HRID 474187 の反応式
[CH2:1]([S:8][C:9]1[C:10](=[O:17])[N:11]([CH2:15][CH3:16])[CH:12]=[CH:13][N:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Na].S([O-])(O[O-])(=O)=[O:20].[K+].[K+].[OH2:27]>O1CCCC1>[CH2:1]([S:8]([C:9]1[C:10](=[O:17])[N:11]([CH2:15][CH3:16])[CH:12]=[CH:13][N:14]=1)(=[O:20])=[O:27])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 5360545SodiumHCID 10313463Potassium peroxymonosulphateHCID 44218624HCID 44218624、化合物

生成物 1

HCID 44218625HCID 44218625、化合物収率 52%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 177 mg (0.72 mM) of 3-(benzylthio)-1-ethylpyrazin-2(1H)-one and 66.4 mg (0.79 mM) of sodium hydrogenocarbonate in 4 ml of tetrahydrofurane were added 1.67 g (2.87 mM) of potassium peroxymonosulfate (oxone) in 4 ml of water. The reaction mixture was then stirred at room temperature for 16 h. Water was added and the organic phase was extracted twice with ethyle acetate. The combined organic layer was washed with water, dried on anhydrous sodium sulfate and the solvent was removed under vacuum, to give a solid, which was triturated in diisopropyle oxide, filtrated and dried under vacuum, to give 103 mg of 3-benzylsulfonyl-1-ethylpyrazin-2(1H)-one. Yield: 52%.

後処理

  1. extractionthe organic phase was extracted twice with ethyle acetate
  2. washThe combined organic layer was washed with water
  3. dry with materialdried on anhydrous sodium sulfate
  4. customthe solvent was removed under vacuum
  5. customto give a solid, which
  6. customwas triturated in diisopropyle oxide
  7. filtrationfiltrated
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-4564d58fb6044d6790e9d9e76e65c8b6
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08637522B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート