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

HRID 1060893ノート

反応式

HRID 1060893 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-84877310b21f405fb35ba5fe385d4ca8
出典データセット
uspto-grants-2003_02
特許番号
US06525074B2

反応ノート

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