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

HRID 1731044노트

반응식

HRID 1731044 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-785c734401934106a54b46f7f0f1406e
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03994954

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