Heptane → (8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine di-D-tartrate

HRID 2369349ノート

反応式

HRID 2369349 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]2[N:29]=[C:14]3[C@H:15]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[C:25]([F:28])([F:27])[F:26])[CH2:16][CH2:17][CH2:18][N:13]3[N:12]=2)[CH:6]=[CH:5][C:4]=1[N:30]1[CH:34]=[C:33]([CH3:35])[N:32]=[CH:31]1.[C:36]([C@H:39]([C@@H:41]([C:43]([O-:45])=[O:44])[OH:42])[OH:40])([O-:38])=[O:37].CCCCCCC>C(O)(=O)[C@H]([C@@H](C(O)=O)O)O.C(O)C>[C:36]([C@H:39]([C@@H:41]([C:43]([OH:45])=[O:44])[OH:42])[OH:40])([OH:38])=[O:37].[C:36]([C@H:39]([C@@H:41]([C:43]([OH:45])=[O:44])[OH:42])[OH:40])([OH:38])=[O:37].[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]2[N:29]=[C:14]3[C@H:15]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[C:25]([F:28])([F:27])[F:26])[CH2:16][CH2:17][CH2:18][N:13]3[N:12]=2)[CH:6]=[CH:5][C:4]=1[N:30]1[CH:34]=[C:33]([CH3:35])[N:32]=[CH:31]1

参加物

5

反応物 3

HCID 8900HeptaneHCID 5460284D-TartrateHCID 46854987E-2212

生成物 1

HCID 86659212(8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine di-D-tartrate

試薬・触媒・溶媒 1

HCID 86653873D-tartaric acid ethanol溶媒

実験手順

(8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine (810.18 mg) was dissolved in 8 mL of a D-tartaric acid-ethanol solution (751.13 mg/10 mL) with stirring at room temperature. The oil was precipitated when 2 mL of heptane was added. Accordingly, the oily substance was dissolved by ultrasonic treatment to prepare a clear solution. Several mg of crystals of the 1.5 D-tartrate prepared according to Example 1 were added, followed by stirring at room temperature. Stirring for about one hour resulted in gelation and subsequent precipitation of a solid. Further, stirring was continued while gradually adding 14 mL of heptane. A part of the suspension (2 mL) was separated and the solid was collected by filtration through a glass filter. The solid was dried under reduced pressure at room temperature to obtain 71.14 mg of the title compound as white solid crystals.

後処理

  1. customThe oil was precipitated when 2 mL of heptane
  2. additionwas added
  3. dissolutionAccordingly, the oily substance was dissolved by ultrasonic treatment
  4. customto prepare a clear solution
  5. additionwere added
  6. stirringby stirring at room temperature
  7. stirringStirring for about one hour
  8. customresulted in gelation and subsequent precipitation of a solid
  9. stirringFurther, stirring
  10. customA part of the suspension (2 mL) was separated
  11. filtrationthe solid was collected by filtration through a glass
  12. filtrationfilter
  13. customThe solid was dried under reduced pressure at room temperature

出典と根拠

ORDレコード
ord-3d4cbf876ec44f7e8670bf079014ff90
出典データセット
uspto-grants-2014_04
特許番号
US08703954B2

反応ノート

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