2,6-dimethoxy-4-(methoxy-carbonyl)-N-methyl-carbanilic acid benzyl ester → Methyl 3,5-dimethoxy-4-(methylamino)benzoate

HRID 542972ノート

反応式

HRID 542972 の反応式
C(O[C:9](=O)[N:10](C)[C:11]1[C:16]([O:17][CH3:18])=[CH:15][C:14]([C:19]([O:21][CH3:22])=[O:20])=[CH:13][C:12]=1[O:23][CH3:24])C1C=CC=CC=1.[H][H]>CO.[Pd]>[CH3:22][O:21][C:19](=[O:20])[C:14]1[CH:15]=[C:16]([O:17][CH3:18])[C:11]([NH:10][CH3:9])=[C:12]([O:23][CH3:24])[CH:13]=1

参加物

5

反応物 2

HCID 542703972,6-dimethoxy-4-(methoxy-carbonyl)-N-methyl-carbanilic acid benzyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 53774973Methyl 3,5-dimethoxy-4-(methylamino)benzoate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A suspension of 33.5 g. of 2,6-dimethoxy-4-(methoxy-carbonyl)-N-methylcarbanilic acid benzyl ester in 1 liter of methanol was hydrogenated in the presence of 1.5 g. of palladium on carbon (5%) until the hydrogen uptake stopped. The suspension was heated to boiling and filtered. The filtrate was evaporated under vacuum and the residue recrystallized from cyclohexane, whereby there was obtained 3,5-dimethoxy-4-(methylamino)-benzoic acid methyl ester having a melting point of 49°-51° C.

後処理

  1. additionA suspension of 33.5 g
  2. temperatureThe suspension was heated
  3. filtrationfiltered
  4. customThe filtrate was evaporated under vacuum
  5. customthe residue recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-b5a32436cf624014b06623aa79682361
出典データセット
uspto-grants-1987_04
特許番号
US04659818

反応ノート

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