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Water → 2-benzylsulfonyl-7-chloro-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

HRID 703831
ノート
印刷プレビュー

反応式

HRID 703831 の反応式
[CH2:1]([S:8][C:9]1[S:20][C:12]2=[N:13][C:14]([Cl:19])=[C:15]([CH3:18])[C:16](=[O:17])[N:11]2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:21]OS([O-])=O.[K+].[OH2:27]>CO>[CH2:1]([S:8]([C:9]1[S:20][C:12]2=[N:13][C:14]([Cl:19])=[C:15]([CH3:18])[C:16](=[O:17])[N:11]2[N:10]=1)(=[O:21])=[O:27])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 142544222-benzylthio-7-chloro-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-oneHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 142544422-benzylsulfonyl-7-chloro-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one収率 62%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

Four point nine (4.9) grams of 2-benzylthio-7-chloro-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was dissolved in methanol. To this solution, an aqueous suspension of 69.2 g of OXONE® in 240 ml of water was added, and the mixture was stirred at 60° C. for 1 hour and 45 minutes. After cooling, the reaction mixture was extracted with chloroform, the organic layer was washed with an aqueous sodium thiosulfate solution and water respectively and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was recrystallized from a toluene/ethanol (1:1) mixture. Thus 3.3 g of 2-benzylsulfonyl-7-chloro-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 211°-213° C. Yield 62%.

後処理

  1. additionwas added
  2. temperatureAfter cooling
  3. extractionthe reaction mixture was extracted with chloroform
  4. washthe organic layer was washed with an aqueous sodium thiosulfate solution and water respectively
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was recrystallized from a toluene/ethanol (1:1) mixture

出典と根拠

ORDレコード
ord-681c7d0ef5dd4f2eaa6f57932f892484
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04985432

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート