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 1904891

反応式

HRID 1904891 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-afd5f5580a3f40f69947b211027c4b3a
出典データセット
uspto-grants-1989_06
特許番号
US04840883

関連ノート

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