Hydrochloric Acid → HCID 178463795, 화합물

HRID 244525

반응식

HRID 244525 반응식
[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]

참가 물질

7

반응물 4

HCID 313Hydrochloric Acid2회HCID 7120N,N-Diethyl-p-phenylenediamineHCID 24502Potassium DichromateHCID 13796402N-[3-(dimethylamino)phenyl]methanesulphonamide

생성물 1

HCID 178463795HCID 178463795, 화합물수율 22%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-62fc057aeeea43c299d1f805d62a92e3
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658665B2

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