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Methanethiol → N-[(5-chloro-4,6-dimethylpyrimidin-2-yl)aminocarbonyl]-2-(methylthio)carbonylbenzenesulfonamide

HRID 2295246
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HRID 2295246 반응식
C[Al](C)C.[Cl:5][C:6]1[C:7]([CH3:30])=[N:8][C:9]([NH:13][C:14]([NH:16][S:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[C:26](OC)=[O:27])(=[O:19])=[O:18])=[O:15])=[N:10][C:11]=1[CH3:12].[CH3:31][SH:32]>C1(C)C=CC=CC=1>[Cl:5][C:6]1[C:7]([CH3:30])=[N:8][C:9]([NH:13][C:14]([NH:16][S:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[C:26]([S:32][CH3:31])=[O:27])(=[O:19])=[O:18])=[O:15])=[N:10][C:11]=1[CH3:12]
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참가 물질

5

반응물 3

HCID 878MethanethiolHCID 13038397N-[(5-chloro-4,6-dimethylpyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamideHCID 16682925Trimethylaluminum

생성물 1

HCID 13305297N-[(5-chloro-4,6-dimethylpyrimidin-2-yl)aminocarbonyl]-2-(methylthio)carbonylbenzenesulfonamide

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Trimethylaluminum (6.0 ml, 2 M) is charged via syringe to 15 ml dry toluene under nitrogen atmosphere and 3.8 g N-[(5-chloro-4,6-dimethylpyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide is added portionwise. After stirring at room temperature for one hour, methyl mercaptan (gas) is passed through the reaction mixture until the initial temperature rise subsided, whereupon the addition is discontinued. The reaction mixture is allowed to stir at room temperature for 1 hour, and quenched with 25 ml of 10% HCl. The resultant white suspension is filtered to give the desired product.

후처리

  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 is filtered

출처 및 근거

ORD 기록
ord-a57b883dc4414a7387d0188c9cecc6d4
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04424073

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