Benzamide, N-(5-chloro-2-hydroxy-4-nitrophenyl)- → Benzamide, N-(4-amino-5-chloro-2-hydroxyphenyl)-

HRID 1904886

反応式

HRID 1904886 の反応式
[C:1]([NH:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([N+:17]([O-])=O)=[CH:12][C:11]=1[OH:20])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)C.[Pd]>[C:1]([NH:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([NH2:17])=[CH:12][C:11]=1[OH:20])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 1

HCID 5483228Benzamide, N-(5-chloro-2-hydroxy-4-nitrophenyl)-

生成物 1

HCID 78779Benzamide, N-(4-amino-5-chloro-2-hydroxyphenyl)-

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 28 g (96×10-3 mole) of 2-benzamido-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. 26 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-65598d31e3154819a861ae1e3f47c46f
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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