Acetone → sodium;(E)-7-[3-(4-fluorophenyl)-1-propan-2-ylindol-2-yl]-3,5-dihydroxyhept-6-enoate

HRID 2219846

반응식

HRID 2219846 반응식
[CH3:1][CH:2]([N:4]1[C:12](/[CH:13]=[CH:14]/[CH:15]([OH:23])[CH2:16][CH:17]([OH:22])[CH2:18][C:19]([OH:21])=[O:20])=[C:11]([C:24]2[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=2)[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]1=2)[CH3:3].[OH-].[Na+:32].CC(C)=O>CO>[CH3:3][CH:2]([N:4]1[C:12](/[CH:13]=[CH:14]/[CH:15]([OH:23])[CH2:16][CH:17]([OH:22])[CH2:18][C:19]([O-:21])=[O:20])=[C:11]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]1=2)[CH3:1].[Na+:32]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 5353627(6E)-7-(3-(4-fluorophenyl)-1-(propan-2-yl)-1H-indol-2-yl)-3,5-dihydroxyhept-6-enoic acid

생성물 1

HCID 16760425sodium;(E)-7-[3-(4-fluorophenyl)-1-propan-2-ylindol-2-yl]-3,5-dihydroxyhept-6-enoate수율 62%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Fluvastatin (3 g) was completely dissolved in MeOH (15 ml) at reflux temperature. Then, the solution was filtered to obtain a clear solution and heated to reflux again. NaOH (s) (0.29 g) was added at reflux temperature to obtain a precipitate. The slurry was cooled to room temperature to obtain a paste-like mixture. Acetone (30 g) was added dropwise at room temperature and the solution stirred at room temperature for 21 h to obtain a massive precipitate. The product was filtered under nitrogen flow, washed with acetone (2×15 ml) and dried at 50° C. in a vacuum oven for 22.5 h to obtain 1.89 g (62%) of fluvastatin sodium Form XLVIII.

후처리

  1. temperatureat reflux temperature
  2. filtrationThen, the solution was filtered
  3. customto obtain a clear solution
  4. temperatureheated
  5. temperatureto reflux again
  6. temperatureat reflux temperature
  7. customto obtain a precipitate
  8. customto obtain a paste-like mixture
  9. customto obtain a massive precipitate
  10. filtrationThe product was filtered under nitrogen flow
  11. washwashed with acetone (2×15 ml)
  12. customdried at 50° C. in a vacuum oven for 22.5 h

출처 및 근거

ORD 기록
ord-f2341bb8e61d4ca48c6469e1f07324c7
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07414140B2

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