Sodium Carbonate → N-Boc-4-Hydroxyphenyl-DL-glycine

HRID 1731044ノート

反応式

HRID 1731044 の反応式
C([O:5][C:6](=[O:23])[CH:7]([C:16]1[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=1)[NH:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])CCC.C(=O)([O-])[O-].[Na+].[Na+]>CO>[C:12]([O:11][C:9]([NH:8][CH:7]([C:16]1[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=1)[C:6]([OH:23])=[O:5])=[O:10])([CH3:15])([CH3:13])[CH3:14]

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 20312394N-t-butoxycarbonyl-2-(4-hydroxyphenyl)glycine n-butyl ester

生成物 1

HCID 4189925N-Boc-4-Hydroxyphenyl-DL-glycine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 0.5 g. (1.5 mmol.) of N-t-butoxycarbonyl-2-(4-hydroxyphenyl)glycine n-butyl ester in 20 ml. of methanol and 30 ml. of 5% aqueous sodium carbonate was heated at reflux for 30 minutes. The solvent was removed in vacuo and the aqueous residue was extracted with ethyl acetate. The aqueous phase was acidified to pH 3.0 with phosphoric acid and again extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated to give N-t-butoxycarbonyl-2-(4-hydroxyphenyl)glycine, m.p. 112°-114° (methanol-water).

後処理

  1. temperatureat reflux for 30 minutes
  2. customThe solvent was removed in vacuo
  3. extractionthe aqueous residue was extracted with ethyl acetate
  4. extractionagain extracted with ethyl acetate
  5. dry with materialThe extract was dried (Na2SO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-785c734401934106a54b46f7f0f1406e
出典データセット
uspto-grants-1976_11
特許番号
US03994954

反応ノート

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