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Ammonium Chloride → 2-Amino-4-methoxy-5-(2-methoxyethoxy)benzamide

HRID 61663
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반응식

HRID 61663 반응식
[CH3:1][O:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[C:5]([N+:17]([O-])=O)[CH:4]=1.[NH4+].[Cl-]>COCCOC.CO.[Pd]>[NH2:17][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[C:11]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[CH:10][C:6]=1[C:7]([NH2:9])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 593618834-Methoxy-5-(2-methoxyethoxy)-2-nitrobenzamide

생성물 1

HCID 593619522-Amino-4-methoxy-5-(2-methoxyethoxy)benzamide

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of 4-methoxy-5-(2-methoxyethoxy)-2-nitrobenzamide (4.5 g, contains some NH4Cl) and 10% Pd/C (ca. 0.5 g) in DME (200 mL) and MeOH (200 mL) was hydrogenated under a balloon of H2 at RT for 12 h. The mixture was filtered through a pad of Celite® and concentrated in vacuo to give 2-amino-4-methoxy-5-(2-methoxyethoxyl)benzamide as an off white solid (2.8 g, 11.6 mmol). HPLC retention time 2.80 mins.

후처리

  1. filtrationThe mixture was filtered through a pad of Celite®
  2. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fe0db70c450c42e391bd0ddb90fa164e
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440961B2

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