Methanol → p-Hydroxyphenylglycine methyl ester

HRID 2084893

反応式

HRID 2084893 の反応式
S(Cl)(Cl)=O.[CH:5]1[C:10]([C@@H:11]([NH2:15])[C:12]([OH:14])=[O:13])=[CH:9][CH:8]=[C:7]([OH:16])[CH:6]=1.[CH3:17]O>>[CH3:17][O:13][C:12](=[O:14])[CH:11]([NH2:15])[C:10]1[CH:9]=[CH:8][C:7]([OH:16])=[CH:6][CH:5]=1

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 89853D-p-hydroxyphenylglycine

生成物 1

HCID 4123006p-Hydroxyphenylglycine methyl ester

実験手順

To 50 mL of methanol cooled to 0° C. was dropwise added 3.75 mL of thionyl chloride followed by 5.0 g (0.030 mmol) of D-4-hydroxyphenylglycine. The reaction was heated to reflux for 5 h then stirred overnight at room temperature. The resulting mixture was concentrated in vacuo and the residue was diluted with ether. The resulting solid was collected by filtration and dried in vacuo to provide 5.9 g of amino-(4-hydroxy-phenyl)-acetic acid methyl ester as a white solid. Electrospray Mass Spec 182.2 (M+H)+.

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 5 h
  3. concentrationThe resulting mixture was concentrated in vacuo
  4. additionthe residue was diluted with ether
  5. filtrationThe resulting solid was collected by filtration
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-0804f6a6f7354148916932b9c6cce5f3
出典データセット
uspto-grants-2004_04
特許番号
US06716833B2

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