Dimethylformamide → N-[[[2-(chlorosulphonyl)-4-methoxyphenyl]amino]methylene]-N-methyl-methanaminium chloride

HRID 882715

반응식

HRID 882715 반응식
[CH3:1][N:2]([CH3:5])[CH:3]=O.[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][C:8]=1[S:15]([OH:18])(=O)=[O:16].S(Cl)([Cl:21])=O>C1(C)C=CC=CC=1>[Cl-:21].[Cl:21][S:15]([C:8]1[CH:9]=[C:10]([O:13][CH3:14])[CH:11]=[CH:12][C:7]=1[NH:6][CH:3]=[N+:2]([CH3:5])[CH3:1])(=[O:18])=[O:16]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 832602-Amino-5-methoxybenzenesulfonic acid

생성물 1

HCID 86645616N-[[[2-(chlorosulphonyl)-4-methoxyphenyl]amino]methylene]-N-methyl-methanaminium chloride

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

Dimethylformamide (0.152 mol) is added dropwise to a suspension of 2-amino-5-methoxybenzenesulphonic acid (0.152 mol) in thionyl chloride (0.763 mol). The reaction mixture is heated very gradually to 70° C. and is maintained at that temperature for 1.5 hours. After cooling, the stirred reaction solution is treated by the addition of 20 ml of toluene. A precipitate is formed which is rapidly filtered off, rinsed with toluene and then dried at 40° C. in vacuo in the presence of KOH pellets, to yield the title product.

후처리

  1. temperatureis maintained at that temperature for 1.5 hours
  2. temperatureAfter cooling
  3. customthe stirred reaction solution
  4. customA precipitate is formed which
  5. filtrationis rapidly filtered off
  6. washrinsed with toluene
  7. dry with materialdried at 40° C. in vacuo in the presence of KOH pellets

출처 및 근거

ORD 기록
ord-2d6f4484f9314edbbd2af6e7144af055
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236790B2

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