Potassium Carbonate → 4-{2-[3-(3-Thieno[2,3-d]isoxazol-3-yl-phenoxy)-propylamino]-ethyl}-benzenesulfonamide

HRID 8656

반응식

HRID 8656 반응식
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([C:12]2[C:16]3[S:17][CH:18]=[CH:19][C:15]=3[O:14][N:13]=2)[CH:9]=[CH:10][CH:11]=1.ClCCCOC1C=C(C2C3SC=CC=3ON=2)C=CC=1.[NH2:39][CH2:40][CH2:41][C:42]1[CH:47]=[CH:46][C:45]([S:48]([NH2:51])(=[O:50])=[O:49])=[CH:44][CH:43]=1.C(=O)([O-])[O-].[K+].[K+]>>[O:14]1[C:15]2[CH:19]=[CH:18][S:17][C:16]=2[C:12]([C:8]2[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=2)[O:5][CH2:4][CH2:3][CH2:2][NH:39][CH2:40][CH2:41][C:42]2[CH:43]=[CH:44][C:45]([S:48]([NH2:51])(=[O:49])=[O:50])=[CH:46][CH:47]=2)=[N:13]1

참가 물질

5

반응물 4

HCID 11430Potassium CarbonateHCID 1696824-(2-Aminoethyl)benzenesulfonamideHCID 219835563-[3-(3-Chloro-propoxy)-phenyl]-thieno[2,3-d]isoxazoleHCID 219835593-[3-(3-Bromo-propoxy)phenyl]-thieno[2,3-d]isoxazole

생성물 1

HCID 99119814-{2-[3-(3-Thieno[2,3-d]isoxazol-3-yl-phenoxy)-propylamino]-ethyl}-benzenesulfonamide수율 35%

실험 절차

The title compound is prepared from a mixture of 3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole, 3-[3-(3-chloro-propoxy)-phenyl]-thieno[2,3-d]isoxazole, 4-(2-aminoethyl) benzenesulfonamide and potassium carbonate essentially as described above in example 4 except that the column is eluted using a graded solvent mixture of dichloromethane:methanol (90:10). Combine the appropriate fractions and concentrate to give the title compound (0.16 g, 35% Yield) as a solid. Purity by LC/MS (APCI)=96% area, [M+H]+=458 m/e.

후처리

  1. washis eluted
  2. additiona graded solvent mixture of dichloromethane:methanol (90:10)
  3. concentrationCombine the appropriate fractions and concentrate

출처 및 근거

ORD 기록
ord-35056de0b49747e79ad154c41ebc6c38
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091199B1

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