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

HRID 1777574ノート

反応式

HRID 1777574 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 232051694-(Methyl(phenyl)amino)benzoic acid収率 40%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9bf10752906741ec9a68190ae6791deb
出典データセット
uspto-grants-2016_02
特許番号
US09266832B2

反応ノート

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