Methyl iodide → 4-(Methyl(phenyl)amino)benzoic acid

HRID 1777574노트

반응식

HRID 1777574 반응식
[H-].[Na+].[C:3]1([NH:9][C:10]2[CH:19]=[CH:18][C:13]([C:14]([O:16]C)=[O:15])=[CH:12][CH:11]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:20]I>C1COCC1.O>[CH3:20][N:9]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)[C:10]1[CH:19]=[CH:18][C:13]([C:14]([OH:16])=[O:15])=[CH:12][CH:11]=1

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 614877Methyl 4-anilinobenzoate

생성물 1

HCID 232051694-(Methyl(phenyl)amino)benzoic acid수율 40%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

NaH 60% dispersed in mineral oil (0.030 g; 0.745 mmol) was added to a solution of methyl 4-(phenylamino)benzoate (0.113 g; 0.497 mmol) in THF (3 mL). After stirring the resulting solution for 10 minutes, methyl iodide (0.062 mL; 0.994 mmol) was added and the resulting mixture was stirred overnight at room temperature. The mixture was diluted in water and extracted with ethyl acetate. The organic layer was washed with brine and dried to yield 0.045 g (40%) of the title compound as a white solid.

후처리

  1. stirringthe resulting mixture was stirred overnight at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. customdried

출처 및 근거

ORD 기록
ord-9bf10752906741ec9a68190ae6791deb
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266832B2

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