Hydrazine hydrate (1:1) → N-(5-aminoacetylamino-4-nitro-2-phenoxyphenyl)methanesulfonamide

HRID 441127노트

반응식

HRID 441127 반응식
[N+:1]([C:4]1[C:9]([NH:10][C:11](=[O:24])[CH2:12][N:13]2C(=O)C3=CC=CC=C3C2=O)=[CH:8][C:7]([NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[C:6]([O:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:5]=1)([O-:3])=[O:2].O.NN>ClCCl.CO>[NH2:13][CH2:12][C:11]([NH:10][C:9]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]([O:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:7]([NH:25][S:26]([CH3:29])(=[O:27])=[O:28])[CH:8]=1)=[O:24]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 22406108N-(4-nitro-2-phenoxy-5-phthalimidoacetylaminophenyl)methanesulfonamide

생성물 1

HCID 22406110N-(5-aminoacetylamino-4-nitro-2-phenoxyphenyl)methanesulfonamide수율 73.5%

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

To 350 ml of a dichloromethane-methanol (5:2) solution containing 9.5 g of N-(4-nitro-2-phenoxy-5-phthalimidoacetylaminophenyl)methanesulfonamide was added 0.64 ml of 99% hydrazine monohydrate at room temperature, followed by stirring for 19 hours. The precipitate was removed by filtration, followed by washing with hot acetonitrile. The filtrate was washed with water, and concentrated under reduced pressere. The resulting precipitate was washed with ethanol and dried to give 5.2 g of N-(5-aminoacetylamino-4-nitro-2 -phenoxyphenyl)methanesulfonamide as yellow crystals.

후처리

  1. customThe precipitate was removed by filtration
  2. washby washing with hot acetonitrile
  3. washThe filtrate was washed with water
  4. concentrationconcentrated under reduced pressere
  5. washThe resulting precipitate was washed with ethanol
  6. customdried

출처 및 근거

ORD 기록
ord-a8948d2e22914161856ac9ca49e3a941
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521311

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