Citric Acid → N-Methyl-N-phenyl-glycine

HRID 2184087

反応式

HRID 2184087 の反応式
[CH3:1][N:2]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:3][C:4]([O:6]CC)=[O:5].[OH-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CO>[CH3:1][N:2]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:3][C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 311Citric AcidHCID 14798Sodium HydroxideHCID 265936(Methyl-phenyl-amino)-acetic acid ethyl ester

生成物 1

HCID 420843N-Methyl-N-phenyl-glycine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The product of step 1 (1.1 g, 5.6 mmol) was dissolved in methanol (50 mL) and 1M NaOH (17 mL) added. Allow reaction mixture to stir at ambient temperature over 18 hours. 10% Citric acid solution was added until a pH=4 was reached. Extract several times with EtOAc. The organic layer was washed several times with brine, dried (Na2SO4), filtered, and concentrated affording a quantitative yield of the title compound as a yellow oil. MS (ES+) m/z 166 (MH+).

後処理

  1. customAllow reaction mixture
  2. extractionExtract several times with EtOAc
  3. washThe organic layer was washed several times with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-03fbe0f0d40340a7bc7bf134029aebc9
出典データセット
uspto-grants-2005_05
特許番号
US06900244B2

関連ノート

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