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Water → methyl N-(4,6-dimethylpyrimidin-2-yl)-N'-(2-phenylphenyl)sulfonylcarbamimidothioate

HRID 637869
ノート
印刷プレビュー

反応式

HRID 637869 の反応式
[C:1]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([NH:10][C:11]([NH:13][C:14]1[N:19]=[C:18]([CH3:20])[CH:17]=[C:16]([CH3:21])[N:15]=1)=[S:12])(=[O:9])=[O:8].[Na].[CH3:29]I.O>C(#N)C.C(O)C>[C:1]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([NH:10][C:11](=[N:13][C:14]1[N:15]=[C:16]([CH3:21])[CH:17]=[C:18]([CH3:20])[N:19]=1)[S:12][CH3:29])(=[O:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 5360545SodiumHCID 134885341-(2-Biphenylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)thiourea

生成物 1

HCID 178503865methyl N-(4,6-dimethylpyrimidin-2-yl)-N'-(2-phenylphenyl)sulfonylcarbamimidothioate収率 38.8%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 6342Acetonitrile溶媒

実験手順

3.98 g of 1-(2-biphenylylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)thiourea was suspended in 50 ml of dry acetonitrile, and a solution of 0.3 g of metallic sodium in 10 ml of ethanol was added, and the mixture was heated under reflux for 30 minutes. After cooling, 1.85 g of methyl iodide was added, and the mixture was heated under reflux for 5 hours. The reaction mixture was cooled, and then poured into 100 ml of water. The product was extracted with methylene chloride. Methylene chloride was evaporated under reduced pressure, and the residue was recrystallized from ethanol to give 1.6 g of the desired 1-(2-biphenylylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)2-methylisothiourea (compound No. II-1) which was the same as obtained in Example 1. mp. 154°-157° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. temperatureAfter cooling
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 5 hours
  6. temperatureThe reaction mixture was cooled
  7. extractionThe product was extracted with methylene chloride
  8. customMethylene chloride was evaporated under reduced pressure
  9. customthe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-89bf74d21d564b4b9206beac4d6bd9e5
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04559079

反応ノート

読み込み中…

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