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Citric Acid → N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide

HRID 1648794
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HRID 1648794 반응식
[CH3:1][NH:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)(=[O:5])=[O:4].C([N:15]([CH2:18]C)CC)C.[S:20](Cl)Cl.CN[CH:25]=[N:26][C:27]1[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:28]=1[CH3:34].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O.C(Cl)Cl>[Cl:33][C:31]1[CH:30]=[CH:29][C:28]([CH3:34])=[C:27]([N:26]=[CH:25][CH2:18][NH:15][S:20][N:2]([CH3:1])[S:3]([C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=2)(=[O:4])=[O:5])[CH:32]=1
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참가 물질

8

반응물 5

HCID 311Citric AcidHCID 8471Triethylamine2회HCID 12543N-Methyl-p-toluenesulfonamideHCID 25353Sulfur dichlorideHCID 178484923HCID 178484923, 화합물

생성물 1

HCID 86739104N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide수율 8%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution cooled to -10° of 18.5 g. (0.1 mole) of N-methyl-p-toluenesulfonamide and 10.1 g. (0.1 mole) of triethylamine in 300 ml. of methylene chloride is added dropwise 10.3 g. (0.1 mole) sulfur dichloride. The reaction mixture is stirred at ambient temperature for 0.5 hour and cooled to 10°. A solution of 18.3 g (0.1 mole) of N-methyl-N'-(4-chloro-o-tolyl)formamidine and 10.1 g. (0.1 mole) triethylamine in 100 ml. of methylene chloride is added rapidly with stirring. The reaction mixture is stirred at ambient temperature for 0.5 hour and extracted successively with 300 ml. of water, 300 ml. aqueous citric acid solution containing 10.5 g. (0.05 mole) of citric acid, and 300 ml. of water. The organic layer is dried and the solvent removed under reduced pressure. The residue is chromatographed over 100 g. silica gel using Hexane:Et2O:Et3N (18:2:3 by volume) to obtain 3.2 g. (8% yield) of N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide as a viscous oil.

후처리

  1. temperatureTo a stirred solution cooled to -10° of 18.5 g
  2. temperaturecooled to 10°
  3. stirringwith stirring
  4. stirringThe reaction mixture is stirred at ambient temperature for 0.5 hour
  5. extractionextracted successively with 300 ml
  6. additionaqueous citric acid solution containing 10.5 g
  7. customThe organic layer is dried
  8. customthe solvent removed under reduced pressure
  9. customThe residue is chromatographed over 100 g
  10. customto obtain 3.2 g

출처 및 근거

ORD 기록
ord-32b959f5850741daa9940681b2d38dea
출처 데이터셋
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04413013

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