Hydrochloric Acid → 3-(3-Methoxy-benzenesulfonylamino)-propionic acid

HRID 1060893노트

반응식

HRID 1060893 반응식
C([O:3][C:4](=[O:19])[CH2:5][CH2:6][NH:7][S:8]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[CH:12]=1)(=[O:10])=[O:9])C.[OH-].[Na+].Cl>CCO>[CH3:18][O:17][C:13]1[CH:12]=[C:11]([S:8]([NH:7][CH2:6][CH2:5][C:4]([OH:19])=[O:3])(=[O:10])=[O:9])[CH:16]=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 700249813-(3-Methoxy-benzenesulfonylamino)-propionic acid ethyl ester

생성물 1

HCID 186294403-(3-Methoxy-benzenesulfonylamino)-propionic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-(3-Methoxy-benzenesulfonylamino)-propionic acid ethyl ester (5.62 g, 0.0196 mol) was dissolved in EtOH (200 mL), treated with 1N NaOH solution (20.54 mL), and stirred at ambient temperature for 18 h. The reaction was acidified with 1N HCl to pH<5, the EtOH was removed in vacuo, and the residue was partitioned between EtOAc and H2O. The aqueous layer was washed with EtOAc, the organics combined, washed H2O, brine, and dried (Na2SO4). Filtration and concentration in vacuo gave the title compound. 1H NMR (CDCl3) δ 7.37-7.46 (m, 3H), 7.09-7.13 (m, 1H), 5.82 (t, 1H, J=7 Hz), 3.87 (s, 3H), 3.2-3.3 (m, 2H), 2.63 (t, 2H, J=6 Hz).

후처리

  1. customthe EtOH was removed in vacuo
  2. customthe residue was partitioned between EtOAc and H2O
  3. washThe aqueous layer was washed with EtOAc
  4. washwashed H2O, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationFiltration and concentration in vacuo

출처 및 근거

ORD 기록
ord-84877310b21f405fb35ba5fe385d4ca8
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525074B2

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