2-((2-Methoxyethoxy)methoxy)-3-nitrobenzoic acid methyl ester → 3-Amino-2-((2-methoxyethoxy)methoxy)benzoic acid methyl ester

HRID 912429ノート

反応式

HRID 912429 の反応式
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-])=O)[C:5]=1[O:13][CH2:14][O:15][CH2:16][CH2:17][O:18][CH3:19].[H][H]>CO.[Pd]>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH2:10])[C:5]=1[O:13][CH2:14][O:15][CH2:16][CH2:17][O:18][CH3:19]

参加物

5

反応物 2

HCID 582228052-((2-Methoxyethoxy)methoxy)-3-nitrobenzoic acid methyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 582228163-Amino-2-((2-methoxyethoxy)methoxy)benzoic acid methyl ester収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of 2-((2-methoxyethoxy)methoxy)-3-nitrobenzoic acid methyl ester 5.0 g (17.5 mmol) of step 1 in methanol 50 mL was added 5% Pd/C 0.5 g, and the reactor was filled with hydrogen gas, after which the reaction mixture was stirred at room temperature for 24 hrs. The catalyst was removed off by celite filtration before concentrating the reaction mixture in a vacuum. Purification by column chromatography (developing solvent: ethylacetate/hexane=1/1) afforded 4.2 g of the title compound (yield 95%).

後処理

  1. customThe catalyst was removed off by celite filtration
  2. concentrationbefore concentrating the reaction mixture in a vacuum
  3. customPurification by column chromatography (developing solvent: ethylacetate/hexane=1/1)

出典と根拠

ORDレコード
ord-5d60db39c2664666aa2039d962a96918
出典データセット
uspto-grants-2011_09
特許番号
US08026235B1

反応ノート

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