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

HRID 882715

反応式

HRID 882715 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2d6f4484f9314edbbd2af6e7144af055
出典データセット
uspto-grants-2012_08
特許番号
US08236790B2

関連ノート

読み込み中…