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Methanethiol → HCID 20041818、化合物

HRID 844939
ノート
印刷プレビュー

反応式

HRID 844939 の反応式
C[Al](C)C.[CH3:5][O:6][C:7]1[CH:12]=[C:11]([CH3:13])[NH:10][N:9]([NH:14][C:15]([NH:17][S:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]([O:29]C)=O)(=[O:20])=[O:19])=[O:16])[N:8]=1.[CH3:31][SH:32]>C1(C)C=CC=CC=1>[CH3:5][O:6][C:7]1[CH:12]=[C:11]([CH3:13])[NH:10][N:9]([NH:14][C:15]([NH:17][S:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]([S:32][CH3:31])=[O:29])(=[O:20])=[O:19])=[O:16])[N:8]=1
参加物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 878MethanethiolHCID 16682925TrimethylaluminumHCID 20041811HCID 20041811、化合物

生成物 1

HCID 20041818HCID 20041818、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Trimethylaluminum (6.0 ml, 2M) was charged via syringe to 15 ml dry toluene under nitrogen atmosphere and 3.8 g N-[(4-methoxy-6-methyltriazin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide was added portionwise. After stirring at room temperature for one hour, methyl mercaptan (gas) was passed through the reaction mixture until the initial temperature rise subsided, whereupon the addition was discontinued. The reaction mixture was allowed to stir at room temperature for 1 hour, and quenched with 25 ml of 10% HCl. The resultant white suspension was filtered to give 2.9 g white solid which showed infrared absorption peaks at 1740, 1690 cm-1, consistent for N-[(4-methoxy-6-methyltriazin-2-yl)aminocarbonyl]-2-(methylthio)carbonylbenzenesulfonamide.

後処理

  1. additionsubsided, whereupon the addition
  2. stirringto stir at room temperature for 1 hour
  3. customquenched with 25 ml of 10% HCl
  4. filtrationThe resultant white suspension was filtered

出典と根拠

ORDレコード
ord-7da53eec449247b9a46179d997bf7d7d
出典データセット
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04755216

反応ノート

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