Sodium Hydroxide → Pitavastatin

HRID 451225

反応式

HRID 451225 の反応式
CC([O:5][C:6]([CH2:8][CH:9]([OH:35])[CH2:10][CH:11]([OH:34])[CH:12]=[CH:13][C:14]1[C:23]([CH:24]2[CH2:26][CH2:25]2)=[N:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]=1[C:27]1[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=1)=[O:7])(C)C.[OH-].[Na+]>CO.O>[CH:18]1[CH:19]=[CH:20][C:21]2[N:22]=[C:23]([CH:24]3[CH2:26][CH2:25]3)[C:14](/[CH:13]=[CH:12]/[C@@H:11]([OH:34])[CH2:10][C@@H:9]([OH:35])[CH2:8][C:6]([OH:7])=[O:5])=[C:15]([C:27]3[CH:28]=[CH:29][C:30]([F:33])=[CH:31][CH:32]=3)[C:16]=2[CH:17]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 53395166(3R,5S,E)-tert-butyl 7-(2-cyclopropyl-4-(4-fluorophenyl)quinolin-3-yl)-3,5-dihydroxyhept-6-enoate

生成物 1

HCID 5282452Pitavastatin

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

From pitavastatin tertiary butyl ester: 50 g of pitavastatin tert-butyl ester was taken in 250 ml of methanol and stirred for 10 minutes at 25° C. 6 g of sodium hydroxide is dissolved in 60 ml of water and slowly added to the reaction mixture. Stirred the reaction mixture to 2 hrs at 25°. Distilled off the solvent completely under reduced pressure. To the obtained solid added 50 ml of dichloro methane and stirred for 10 minutes. Cooled the reaction mixture to 0° C. and adjusted the pH to 3.0 with 20% aqueous HCl solution. 60 g of sodium chloride is added to the reaction mixture and stirred for 15 minutes. Raised the temperature to 25° C. and stirred for 30 minutes. Filtered the solid precipitated. Water was added to the solid and stirred for 10 minutes. Filtered the solid and washed with water. Dried the obtained solid to get the title compound.

後処理

  1. additionslowly added to the reaction mixture
  2. stirringStirred the reaction mixture to 2 hrs at 25°
  3. distillationDistilled off the solvent completely under reduced pressure
  4. additionTo the obtained solid added 50 ml of dichloro methane
  5. stirringstirred for 10 minutes
  6. temperatureCooled the reaction mixture to 0° C.
  7. addition60 g of sodium chloride is added to the reaction mixture
  8. stirringstirred for 15 minutes
  9. temperatureRaised the temperature to 25° C.
  10. stirringstirred for 30 minutes
  11. filtrationFiltered the solid
  12. customprecipitated
  13. additionWater was added to the solid
  14. stirringstirred for 10 minutes
  15. filtrationFiltered the solid
  16. washwashed with water
  17. customDried the obtained solid

出典と根拠

ORDレコード
ord-6a6682c4fcb44764b53d85966e8b66c9
出典データセット
uspto-grants-2013_07
特許番号
US08487105B2

関連ノート

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