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2-Nitro-3-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-6-benzamidophenol → 2-Amino-3-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-6-benzamidophenol

HRID 1904889
ノート
印刷プレビュー

反応式

HRID 1904889 の反応式
[N+:1]([C:4]1[C:9]([NH:10][C:11](=[O:32])[CH:12]([O:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]([CH2:25][CH3:26])([CH3:24])[CH3:23])=[CH:18][C:17]=2[C:27]([CH2:30][CH3:31])([CH3:29])[CH3:28])[CH2:13][CH3:14])=[C:8]([Cl:33])[CH:7]=[C:6]([NH:34][C:35](=[O:42])[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[C:5]=1[OH:43])([O-])=O>O1CCCC1.C(O)C.[Pd]>[NH2:1][C:4]1[C:9]([NH:10][C:11](=[O:32])[CH:12]([O:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]([CH2:25][CH3:26])([CH3:23])[CH3:24])=[CH:18][C:17]=2[C:27]([CH2:30][CH3:31])([CH3:29])[CH3:28])[CH2:13][CH3:14])=[C:8]([Cl:33])[CH:7]=[C:6]([NH:34][C:35](=[O:42])[C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[C:5]=1[OH:43]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 200362042-Nitro-3-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-6-benzamidophenol

生成物 1

HCID 200362022-Amino-3-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-6-benzamidophenol

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 50 ml of tetrahydrofuran and 100 ml of ethanol was dissolved 21 g (13×10-3 mole) of 2-nitro-3-{2-(2,4-di-t-amylphenoxy)butanamido}-4-chloro-6-benzamidophenol and hydrogenation was effected by using 1.2 g of Pd-C as a catalyst. The color of the nitro derivative disappeared in 4 hours, and the Pd-C was removed by filtration and a solvent was evaporated therefrom under reduced pressure, 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. Yield: 20 g.

後処理

  1. customthe Pd-C was removed by filtration
  2. customa solvent was evaporated
  3. extractionunder reduced pressure, followed 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

出典と根拠

ORDレコード
ord-dd4333fae6384d24b38f088df7df0e08
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04840883

反応ノート

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