Methanesulfonic Acid → 934240-35-4

HRID 1099012노트

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HRID 1099012 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

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온도
60 °C

실험 절차

EtOAc (6 ml) was added to (5R)-5-(4-{[(2-Fluorophenyl)methyl]oxy}phenyl)-L-prolinamide (E1, 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-3f37ee2af1bd44948f8398803b6227c2
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143306B2

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