Triethylamine → 3-(3-Methoxy-benzenesulfonylamino)-propionic acid ethyl ester

HRID 1060892노트

반응식

HRID 1060892 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([S:9](Cl)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.CCN(CC)CC.Cl.[CH2:21]([O:23][C:24](=[O:28])[CH2:25][CH2:26][NH2:27])[CH3:22]>CC(C)=O>[CH2:21]([O:23][C:24](=[O:28])[CH2:25][CH2:26][NH:27][S:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)(=[O:11])=[O:10])[CH3:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 27375043-Methoxybenzenesulfonyl chloride

생성물 1

HCID 700249813-(3-Methoxy-benzenesulfonylamino)-propionic acid ethyl ester

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

m-Methoxybenzenesulfonyl chloride (3.53 g, 0.017 mol) and Et3N (4.76 mL, 0.034 mol) were dissolved in acetone (35 mL) at 0° C. β-Alanine ethyl ester hydrochloride (2.0 g, 0.017 mol) was added and stirring was continued at room temperature under N2 for 0.5 h. The reaction mixture was concentrated, partitioned between 0.1N HCl solution and EtOAc. The aqueous layer was washed with EtOAc, the organics combined, washed with H2O, brine, and dried (Na2SO4). Filtration and concentration to dryness gave the title compound which was used without further purification.

후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated
  3. custompartitioned between 0.1N HCl solution and EtOAc
  4. washThe aqueous layer was washed with EtOAc
  5. washwashed with H2O, brine
  6. dry with materialdried (Na2SO4)
  7. filtrationFiltration and concentration to dryness

출처 및 근거

ORD 기록
ord-de8b4f98ef9543a59bc13e92e726d2e5
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525074B2

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