Hydrazine hydrate (1:1) → 4-amino-N-methylbenzene-1-sulfonamide

HRID 57231

反応式

HRID 57231 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([N-:13][CH3:14])(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-])=O.O.NN>C(O)C.[Ni]>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([S:10]([NH:13][CH3:14])(=[O:12])=[O:11])=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 866087554-Nitrobenzenesulfonyl methylamide

生成物 1

HCID 743684-amino-N-methylbenzene-1-sulfonamide

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

To a solution of the crude 4-nitrobenzenesulfonyl methylamide prepared above in 45 mL of ethanol, was added a 1 mL slurry of Raney Nickel. Hydrazine monohydrate (18 mmol) was added slowly in several portions. A change in the solution colour from yellow to colourless indicated the reaction was complete. The mixture was stirred for an additional 1 hr. The solids were removed by filtration and the solvent was evaporated. The resulting crude material was purified by flash column chromatography eluting with CH2Cl2:MeOH=10:1 to yield 2.09 g (90% for two steps) of the title compound as a pale orange powder.

後処理

  1. customThe solids were removed by filtration
  2. customthe solvent was evaporated
  3. customThe resulting crude material was purified by flash column chromatography
  4. washeluting with CH2Cl2

出典と根拠

ORDレコード
ord-2af18a93124e4b66859e501bec395da1
出典データセット
uspto-grants-2016_09
特許番号
US09434720B2

関連ノート

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