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

HRID 2098394노트

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HRID 2098394 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 160422955-Amino-2-ethoxy-N-hydroxybenzamide수율 726%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94e415deb1494797ae731a4d9cf908e1
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450506B2

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