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Sodium Hydroxide → Pitavastatin

HRID 451225
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HRID 451225 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 53395166Tert-butyl 7-[2-cyclopropyl-4-(4-fluorophenyl)quinolin-3-yl]-3,5-dihydroxyhept-6-enoate

생성물 1

HCID 5282452Pitavastatin

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a6682c4fcb44764b53d85966e8b66c9
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08487105B2

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