Methanesulfonic Acid → 934240-35-4

HRID 2264847노트

반응식

HRID 2264847 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C@@H:16]2[NH:20][C@H:19]([C:21]([NH2:23])=[O:22])[CH2:18][CH2:17]2)=[CH:12][CH:11]=1.[CH3:24][S:25]([OH:28])(=[O:27])=[O:26]>CCOC(C)=O>[CH3:24][S:25]([OH:28])(=[O:27])=[O:26].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C@@H:16]2[NH:20][C@H:19]([C:21]([NH2:23])=[O:22])[CH2:18][CH2:17]2)=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 16046068(2S,5R)-5-(4-((2-Fluorophenyl)methoxy)phenyl)-2-pyrrolidinecarboxamide

생성물 1

HCID 86624720934240-35-4

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

EtOAc (6 ml) was added to (5R)-5-(4-{[(2-Fluorophenyl)methyl]oxy}phenyl)-L-prolinamide (E4, 300 mg) and this was heated at 60° C. for an hour to dissolve the compound. Then methanesulfonic acid (65 μl, 1.05 eq) was added to the solution and as soon as the acid was added, the solution went cloudy. This was then left to temperature cycle (0-40° C.) for 2 days. The compound was isolated by filtration as a white solid, washed with EtOAc and dried in vacuo at 40° C. overweek-end to afford 335 mg of the title compound.

후처리

  1. dissolutionto dissolve the compound
  2. additionas soon as the acid was added
  3. customThe compound was isolated by filtration as a white solid
  4. washwashed with EtOAc
  5. customdried in vacuo at 40° C. overweek-end

출처 및 근거

ORD 기록
ord-6c9a1843a1864aed8d7e9e96f2895667
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855218B2

반응 노트

불러오는 중…