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

HRID 255301

반응식

HRID 255301 반응식
[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]

참가 물질

4

반응 조건

온도
150 °C

실험 절차

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%)

후처리

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

출처 및 근거

ORD 기록
ord-98808f368c2d4988b537d19cf74e01c2
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875715B2

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