Hydrochloric Acid → HCID 178463795、化合物

HRID 244525

反応式

HRID 244525 の反応式
[CH2:1]([N:3]([CH2:11][CH3:12])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[CH:6][CH:5]=1)[CH3:2].[ClH:13].[CH3:14][N:15]([CH3:27])[C:16]1[CH:17]=[C:18]([NH:22]S(C)(=O)=O)[CH:19]=[CH:20][CH:21]=1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[K+].[K+]>O.CO>[Cl-:13].[CH2:11]([N:3]([CH2:1][CH3:2])[C:4]1[CH:9]=[CH:8][C:7]2[C:6]([CH:5]=1)=[NH+:22][C:18]1[C:19](=[CH:20][CH:21]=[C:16]([N:15]([CH3:27])[CH3:14])[CH:17]=1)[N:10]=2)[CH3:12]

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 7120N,N-Diethyl-p-phenylenediamineHCID 24502Potassium DichromateHCID 13796402N-[3-(dimethylamino)phenyl]methanesulphonamide

生成物 1

HCID 178463795HCID 178463795、化合物収率 22%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

N,N-diethyl-1,4-phenylenediamine (1.00 g, 6.17 mmol) was added slowly to dilute HCl (700 μl, 32%) in H2O (100 cm3). The mixture was stirred until it was homogeneous. N-[3-(dimethylamino)phenyl]methanesulphonamide (1.32 g, 6.17 mmol) in methanol (60 cm3) was added, followed by a saturated aqueous solution of potassium dichromate (2 cm3). The mixture refluxed for 15 min. The mixture was cooled and diluted with water (200 cm3), acidified with hydrochloric acid (1M) and then extracted with chloroform (6×30 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:9 methanol/dichloromethane) gave the target material as a green solid (451 mg, 22%).

後処理

  1. temperatureThe mixture refluxed for 15 min
  2. temperatureThe mixture was cooled
  3. extractionextracted with chloroform (6×30 cm3)
  4. dry with materialThe combined extracts were dried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-62fc057aeeea43c299d1f805d62a92e3
出典データセット
uspto-grants-2014_02
特許番号
US08658665B2

関連ノート

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