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

HRID 441127ノート

反応式

HRID 441127 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21226129Dichloromethane methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a8948d2e22914161856ac9ca49e3a941
出典データセット
uspto-grants-1996_05
特許番号
US05521311

反応ノート

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