Methanol → 5-Amino-2-ethoxy-N-hydroxybenzamide

HRID 1096584ノート

反応式

HRID 1096584 の反応式
[CH2:1]([O:3][C:4]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][C:5]=1[C:6]([NH:8][OH:9])=[O:7])[CH3:2].CO>CCO.[Pd]>[NH2:14][C:11]1[CH:12]=[CH:13][C:4]([O:3][CH2:1][CH3:2])=[C:5]([CH:10]=1)[C:6]([NH:8][OH:9])=[O:7]

参加物

5

反応物 2

HCID 887MethanolHCID 576877782-Ethoxy-N-hydroxy-5-nitrobenzamide

生成物 1

HCID 160422955-Amino-2-ethoxy-N-hydroxybenzamide収率 726%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

2-Ethoxy-5-nitro-N-hydroxybenzamide (2.39 g, 1.06 mmol) was suspended in EtOH (50 ml) and 10% Pd on carbon (wet basis) (240 mg) was added. The mixture was hydrogenated at 50 psi for 1.5 hrs. MeOH (50 ml) was added and the mixture was filtered through celite. The volatiles were removed in vacuo and the residue was taken up in IPA (50 ml). The mixture was heated at 60° C. for 0.5 hr then stood at RT overnight. The precipitated solid was collected by filtration, washed with MTBE and dried in vacuo to give 1.51 g of 5-amino-2-ethoxy-N-hydroxybenzamide (73%) as an off-white solid.

後処理

  1. filtrationthe mixture was filtered through celite
  2. customThe volatiles were removed in vacuo
  3. waitthen stood at RT overnight
  4. filtrationThe precipitated solid was collected by filtration
  5. washwashed with MTBE
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-cc2e67bf8d8244cd868a718149d2cf41
出典データセット
uspto-grants-2012_03
特許番号
US08138357B2

反応ノート

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