Water → Benzoic acid, 3-methoxy-2-nitro-, methyl ester

HRID 576325

反応式

HRID 576325 の反応式
[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[C:15]([O-])([O-])=O.[K+].[K+].CI.O>CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:8][CH3:15])=[O:7]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 786323-Methoxy-2-nitrobenzoic acid

生成物 1

HCID 79195Benzoic acid, 3-methoxy-2-nitro-, methyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 3-methoxy-2-nitrobenzoic acid (25.0 g, 126 mmol) and K2CO3 (35.0 g, 253 mmol) in DMF (126 mL) was added MeI (15.8 mL, 253 mmol) at room temperature. The mixture was stirred at room temperature for 2 hours. To the mixture was poured the water (200 mL) and then stirred at 5° C. for 30 min. The precipitated solid was collected by filtration, washed with water and hexane. The solid was dried under reduced pressure to afford the compound 52 in a crude form (26.2 g, 98%) as a white solid.

後処理

  1. stirringstirred at 5° C. for 30 min
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with water and hexane
  4. customThe solid was dried under reduced pressure

出典と根拠

ORDレコード
ord-fb38c9e1c3204998875316fa067af5e4
出典データセット
uspto-grants-2015_05
特許番号
US09034921B2

関連ノート

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