Potassium Hydroxide → HCID 18786977、化合物

HRID 1107381ノート

反応式

HRID 1107381 の反応式
C([O:3][C:4](=[O:23])[CH2:5][N:6]([CH3:22])[C:7](=[O:21])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:20])C.[OH-].[K+]>CO.O>[CH3:22][N:6]([C:7](=[O:21])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:20])[CH2:5][C:4]([OH:23])=[O:3]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 18786983HCID 18786983、化合物

生成物 1

HCID 18786977HCID 18786977、化合物収率 48.9%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

N-methyl-N-[2-(methylphenyl)benzoyl]glycine ethyl ester (4.5 g, 14.45 mmol) and KOH (2.43 g, 43.4 mmol) in MeOH/H2O (200 mL/50 mL) were heated at reflux for 45 minutes. The solvent was removed and the residue dissolved in H2O. The aqueous solution was washed with Et2O and acidified with HCl (10%). The acidified aqueous layer was extracted with EtOAc, the EtOAc extract was washed with brine (2×), dried over (MgSO4) and evaporated. There was obtained N-methyl-N-[2-(methylphenyl)benzoyl]glycine (2.0 g); LRMS (M+H)+=284.1, (M+NH4)+=301.1

後処理

  1. temperatureat reflux for 45 minutes
  2. customThe solvent was removed
  3. dissolutionthe residue dissolved in H2O
  4. washThe aqueous solution was washed with Et2O
  5. extractionThe acidified aqueous layer was extracted with EtOAc
  6. extractionthe EtOAc extract
  7. washwas washed with brine (2×)
  8. dry with materialdried over (MgSO4)
  9. customevaporated

出典と根拠

ORDレコード
ord-b4ed425bc6bb4fafbf4e415008c9c125
出典データセット
uspto-grants-2000_05
特許番号
US06060462

反応ノート

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