Methanesulfonic Acid → 934240-35-4

HRID 418371ノート

反応式

HRID 418371 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 86624720934240-35-4

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

EtOAc (6 ml) was added to (5R)-5-(4-{[(2-Fluorophenyl)methyl]oxy}phenyl)-L-prolinamide (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.

後処理

  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

出典と根拠

ORDレコード
ord-71890498ccc3479997559a5ad31b5010
出典データセット
uspto-grants-2012_01
特許番号
US08093268B2

反応ノート

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