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N-[3-(acetyl-methyl-amino)-5-amino-phenyl]-N-methyl-acetamide → HCID 19353552, 화합물

HRID 1584211
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인쇄 미리보기

반응식

HRID 1584211 반응식
[C:1]([N:4]([CH3:17])[C:5]1[CH:6]=[C:7]([N:12]([CH3:16])[C:13](=[O:15])[CH3:14])[CH:8]=[C:9]([NH2:11])[CH:10]=1)(=[O:3])[CH3:2].[NH:18]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:19]([CH3:21])=[O:20].[S:28](Cl)(O)(=[O:30])=[O:29]>N1C=CC=CC=1.O>[C:19]([NH:18][C:22]1[CH:27]=[CH:26][C:25]([S:28]([NH:11][C:9]2[CH:8]=[C:7]([N:12]([CH3:16])[C:13](=[O:15])[CH3:14])[CH:6]=[C:5]([N:4]([C:1](=[O:3])[CH3:2])[CH3:17])[CH:10]=2)(=[O:30])=[O:29])=[CH:24][CH:23]=1)(=[O:20])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10776126N-[3-(acetyl-methyl-amino)-5-amino-phenyl]-N-methyl-acetamideHCID 19353479HCID 19353479, 화합물

생성물 1

HCID 19353552HCID 19353552, 화합물수율 55.1%

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

0.15 g (0.00063 mol) of N-[3-(acetyl-methyl-amino)-5-amino-phenyl]-N-methyl-acetamide was dissolved in 3 ml of pyridine, treated with 0.154 g (0.00064 mol) of 4-acetamino-benzene-sulfochloride and stirred at room temperature for 16 hours. Subsequently, the mixture was freed from solvent, the residue was taken up in 25 ml of water, extracted four times with 200 ml of ethyl acetate each time and the combined organic phases were washed with saturated sodium chloride solution and dried over sodium sulfate. After removal of the solvent the residue was chromatographed on silica gel, firstly with 2% and then 5% methanol in dichloromethane. There was obtained 0.15 g (55%) of N-[3-(4-acetylamino-phenylsulfonylamino)-5-(acetyl-methyl-amino)-phenyl]-N-methyl-acetamide as an orange colored, amorphous solid. MS (ISN): me/e=431 (C20H23N4O5S-).

후처리

  1. extractionextracted four times with 200 ml of ethyl acetate each time
  2. washthe combined organic phases were washed with saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent the residue
  5. customwas chromatographed on silica gel, firstly with 2%

출처 및 근거

ORD 기록
ord-0f71de3ff2b04fa3aa176113456c86e0
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05932599

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