N,N'-Dimethylurea → 2-amino-4-fluoro-N-methylbenzamide

HRID 255301

反応式

HRID 255301 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].[CH3:12][NH:13]C(NC)=O>O>[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH:13][CH3:12])=[O:5]

参加物

4

反応物 2

HCID 7293N,N'-DimethylureaHCID 27249674-Fluoroanthranilic acid

生成物 1

HCID 569516612-amino-4-fluoro-N-methylbenzamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of 2-amino 4-fluoro benzoic acid (2.5 g, 16.13 mmol) and 1,3 dimethyl urea (5.85 g, 66.5 mmol) was heated at 150° C. for 24 hours. The reaction was diluted with water, filtered and extracted twice with ethyl acetate. The organic extracts were dried over magnesium sulfate and concentrated at reduced pressure. Chromatography on silica gel with ethyl acetate in hexanes (0-50%) gave the title compound as a waxy solid (670 mg, 25%)

後処理

  1. filtrationfiltered
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-98808f368c2d4988b537d19cf74e01c2
出典データセット
uspto-grants-2011_01
特許番号
US07875715B2

関連ノート

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