반응식
[C:1]1([C@@H](NC(=O)C[C@H](O)C[C@H](O)/C=C/C2N(C(C)C)C3C(C=2C2C=CC(F)=CC=2)=CC=CC=3)C)C=CC=CC=1.[OH-].[Na+:40].[CH:41]1([C:44]2[C:53](/[CH:54]=[CH:55]/[C@@H:56]([OH:64])[CH2:57][C@@H:58]([OH:63])[CH2:59][C:60]([OH:62])=[O:61])=[C:52]([C:65]3[CH:70]=[CH:69][C:68]([F:71])=[CH:67][CH:66]=3)[C:51]3[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=3)[N:45]=2)CC1.Cl>>[Na+:40].[F:71][C:68]1[CH:69]=[CH:70][C:65]([C:52]2[C:51]3[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=3)[N:45]([CH:44]([CH3:1])[CH3:41])[C:53]=2/[CH:54]=[CH:55]/[C@@H:56]([OH:64])[CH2:57][C@@H:58]([OH:63])[CH2:59][C:60]([O-:62])=[O:61])=[CH:66][CH:67]=1참가 물질
실험 절차
can be prepared from (E)-(3R,5S)-7-[3-(4-Fluoro-phenyl)-1-isopropyl-1H-indol-2-yl]-3,5-dihydroxy-hept-6-enoic acid ((S)-1-phenyl-ethyl)-amide by hydrolysis with sodium hydroxide according to the procedure described above for the preparation of (E)-(3R,5S)-7-[2-Cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-3,5-dihydroxy-hept-6-enoic acid. After completion of the hydrolysis, excess sodium hydroxide is neutralised by addition of hydrochloric acid and the solvent is evaporated under reduced pressure. As a work-up variant, the residue is dissolved in water at 60-70° C. and the solution is allowed to cool down to room temperature. Crystallisation occurs. The formed suspension is cooled down to 5° C., stirred for several hours at this temperature to complete the crystallisation and the product is isolated by filtration. (E)-(3R,5S)-7-[3-(4-Fluoro-phenyl)-1-isopropyl-1H-indol-2-yl]-3,5-dihydroxy-hept-6-enoic acid sodium salt is obtained as beige to yellow crystalline product.
후처리
- customthe solvent is evaporated under reduced pressure
- dissolutionAs a work-up variant, the residue is dissolved in water at 60-70° C.
- customCrystallisation
- temperatureThe formed suspension is cooled down to 5° C.
- customthe crystallisation
- customthe product is isolated by filtration
출처 및 근거
- ORD 기록
- ord-ff3e0b23a700424f9ec6ebe4b788f646
- 출처 데이터셋
- uspto-grants-2008_05
- 특허 번호
- US07371865B2
연결된 노트
불러오는 중…