Potassium Carbonate → 2-((2-Methoxyethoxy)methoxy)-3-nitrobenzoic acid methyl ester

HRID 1809130ノート

反応式

HRID 1809130 の反応式
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]=1[OH:13].C([O-])([O-])=O.[K+].[K+].Cl[CH2:22][O:23][CH2:24][CH2:25][O:26][CH3:27]>CN(C)C=O>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]=1[O:13][CH2:22][O:23][CH2:24][CH2:25][O:26][CH3:27]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 775901-(Chloromethoxy)-2-methoxyethaneHCID 596904Methyl 2-hydroxy-3-nitrobenzoate

生成物 1

HCID 582228052-((2-Methoxyethoxy)methoxy)-3-nitrobenzoic acid methyl ester収率 98.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

9.9 g (50 mmol) of 2-hydroxy-3-nitrobenzoic acid methyl ester was dissolved in 100 mL of dimethylformamide. 7.6 g (55 mmol) of K2CO3 and 6.3 mL (55 mmol) of chloromethoxyethoxymethane were added thereto and stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, followed by dilution with ethyl acetate and washing with distilled water and saturated sodium chloride solution. The resulting residue was dried over magnesium sulfate and concentrated under reduced pressure to obtain the title compound (14.0 g, yield: 98%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. washwashing with distilled water and saturated sodium chloride solution
  3. dry with materialThe resulting residue was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d0db3811871d480ba610292ef9464f09
出典データセット
uspto-grants-2013_01
特許番号
US08362012B2

反応ノート

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