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Methanol → 3-[3-(Naphthalen-2-ylsulfamoyl)-phenyl]-acrylic acid

HRID 2180411
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반응식

HRID 2180411 반응식
C[O:2][C:3](=[O:26])[CH:4]=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([S:12](=[O:25])(=[O:24])[NH:13][C:14]2[CH:23]=[CH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=2)[CH:7]=1.CO>>[CH:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:22]=[CH:23][C:14]=1[NH:13][S:12]([C:8]1[CH:7]=[C:6]([CH:5]=[CH:4][C:3]([OH:26])=[O:2])[CH:11]=[CH:10][CH:9]=1)(=[O:24])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 887MethanolHCID 670194963-[3-(Naphthalen-2-ylsulfamoyl)-phenyl]-acrylic acid methyl ester

생성물 1

HCID 670195903-[3-(Naphthalen-2-ylsulfamoyl)-phenyl]-acrylic acid

실험 절차

To a suspension of 3-[3-(naphthalen-2-ylsulfamoyl)-phenyl]-acrylic acid methyl ester (14e) (0.25 g, 0.68 mmol) in methanol (3.5 ml) 2N NaOH solution (1.0 ml, 2.0 mmol) was added and the resultant mixture was stirred at ambient temperature overnight. The reaction mixture was partitioned between ethyl acetate and water. The aqueous layer was acidified with 2N HCl solution and stirred for 30 min. The precipitated solid was filtered, washed with water and dried in desiccator over P2O5. The title compound was obtained as a white solid (0.21 g, 87%). 1H NMR (DMSO-d6, HMDSO), δ: 6.56 (1H, d, J=16.0 Hz); 7.21-8.01 (11H, m); 8.12 (1H, s); 10.56 (1H, br s); 12.54 (1H, br s).

후처리

  1. additionwas added
custom
The reaction mixture was partitioned between ethyl acetate and water
  • filtrationThe precipitated solid was filtered
  • washwashed with water
  • dry with materialdried in desiccator over P2O5
  • 출처 및 근거

    ORD 기록
    ord-6cfb80d911764cc49f4b386cb94271da
    출처 데이터셋
    uspto-grants-2005_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06888027B2

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