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

HRID 1959791노트

반응식

HRID 1959791 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-041e6ab5efa84feba5724f913af97840
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410272B2

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