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Hydrogen Peroxide → 1,3(2H,4H)-Isoquinolinedione, 4,4-dimethyl-2-(2-(methylsulfinyl)ethyl)-

HRID 1448038
ノート
印刷プレビュー

反応式

HRID 1448038 の反応式
OO.[CH3:3][C:4]1([CH3:20])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7](=[O:14])[N:6]([CH2:15][CH2:16][S:17][CH3:18])[C:5]1=[O:19].O.C(=O)([O-])[O-:23]>C(O)(=O)C>[CH3:3][C:4]1([CH3:20])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7](=[O:14])[N:6]([CH2:15][CH2:16][S:17]([CH3:18])=[O:23])[C:5]1=[O:19]
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 784Hydrogen PeroxideHCID 962WaterHCID 19660Carbonate IonHCID 30534781,3(2H,4H)-Isoquinolinedione, 4,4-dimethyl-2-(2-(methylthio)ethyl)-

生成物 1

HCID 30534791,3(2H,4H)-Isoquinolinedione, 4,4-dimethyl-2-(2-(methylsulfinyl)ethyl)-

試薬・触媒・溶媒 1

HCID 176Acetic Acid
溶媒

実験手順

6.9 ml of 30% hydrogen peroxide were added to a solution of 16 gm of 4,4-dimethyl-2-(2-methylmercapto-ethyl)-2H,4H-isoquinoline-1,3-dione in 30 ml of glacial acetic acid, while maintaining the temperature between 20° and 40° C. After 15 minutes the reaction mixture was poured into water, and the resulting mixture was neutralized with ptoassium carbonate and extracted with chloroform. The chloroform phase was evaporated, the residue was purified on a silicagel column (eluant: chloroform/acetone 19:1), and after evaporation of the eluate the residue was recrystallized from cyclohexane by addition of seed crystals.

後処理

  1. temperaturewhile maintaining the temperature between 20° and 40° C
  2. extractionextracted with chloroform
  3. customThe chloroform phase was evaporated
  4. customthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
  5. customafter evaporation of the eluate the residue
  6. customwas recrystallized from cyclohexane by addition of seed crystals

出典と根拠

ORDレコード
ord-311dba5dd39d4f40be76976bc9aa7a38
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04179508

反応ノート

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