2-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-nitrophenol → 2-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-aminophenol

HRID 1904891노트

반응식

HRID 1904891 반응식
[C:1]([C:6]1[CH:29]=[C:28]([C:30]([CH2:33][CH3:34])([CH3:32])[CH3:31])[CH:27]=[CH:26][C:7]=1[O:8][CH:9]([CH2:24][CH3:25])[C:10]([NH:12][C:13]1[CH:18]=[C:17]([Cl:19])[C:16]([N+:20]([O-])=O)=[CH:15][C:14]=1[OH:23])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]>C(O)C.[Pd]>[C:1]([C:6]1[CH:29]=[C:28]([C:30]([CH2:33][CH3:34])([CH3:31])[CH3:32])[CH:27]=[CH:26][C:7]=1[O:8][CH:9]([CH2:24][CH3:25])[C:10]([NH:12][C:13]1[CH:18]=[C:17]([Cl:19])[C:16]([NH2:20])=[CH:15][C:14]=1[OH:23])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]

참가 물질

4

반응물 1

HCID 200361932-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-nitrophenol

생성물 1

HCID 200361922-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-aminophenol

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

In 100 ml of ethanol was dissolved 30 g (61×10-3 mole) of 2-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-5-nitrophenol and hydrogenation was effected by using 1.5 g of Pd-C as a catalyst. The color of the nitro derivative disappeared in 2 hours, and the Pd-C was removed by filtration and ethanol was evaporated from the filtrate, followed by extraction of the residue with ethyl acetate. The ethyl acetate layer was washed with an aqueous sodium hydrogen carbonate solution and then with water, and after drying over magnesium sulfate, ethyl acetate was evaporated. 28 g of the crude product was used as such for the following reaction.

후처리

  1. customthe Pd-C was removed by filtration and ethanol
  2. customwas evaporated from the filtrate
  3. extractionfollowed by extraction of the residue with ethyl acetate
  4. washThe ethyl acetate layer was washed with an aqueous sodium hydrogen carbonate solution
  5. dry with materialwith water, and after drying over magnesium sulfate, ethyl acetate
  6. customwas evaporated
  7. customsuch for the following reaction

출처 및 근거

ORD 기록
ord-afd5f5580a3f40f69947b211027c4b3a
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04840883

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