반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([CH:49]([CH3:51])[CH3:50])[N:11](/[CH:20]=[CH:21]/[C@@H:22]([OH:48])[CH2:23][C:24]([O:26][C@@H:27](C3C=CC=CC=3)C(O)(C3C=CC=CC=3)C3C=CC=CC=3)=[O:25])[C:12]=2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.[Na]>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([CH:49]([CH3:51])[CH3:50])[N:11](/[CH:20]=[CH:21]/[C@@H:22]([OH:48])[CH2:23][C:24]([O:26][CH3:27])=[O:25])[C:12]=2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1참가 물질
반응물 2
생성물 1
시약·촉매·용매 1
실험 절차
A stirred suspension of (S)-1-hydroxy-1,1,2-triphenyleth-2-yl (3S,E)-5-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-3-hydroxy-4-pentenoate (3.11 g) in methanol (30 ml) was treated with a solution of sodium (110 mg) in methanol (20 ml) plus methanol washings (2×5 ml). The resulting orange solution was stirred at room temperature for 2.5 h then the reaction mixture was concentrate. This was dissolved in dichloromethane (150 ml) and the solution was washed with water (50 ml) and brine (2×50 ml). The combined washings were extracted with dichloromethane (50 ml) and the combined organic phases were dried and evaporated to a pale buff solid (3.13 g). This was purified by CC eluting with System A 1:1 to give the title compound (1.588 g) as a white crystalline solid, νmax (nujol) 1738 cm-1 (C=O).
후처리
- concentrationthe reaction mixture was concentrate
- dissolutionThis was dissolved in dichloromethane (150 ml)
- washthe solution was washed with water (50 ml) and brine (2×50 ml)
- extractionThe combined washings were extracted with dichloromethane (50 ml)
- customthe combined organic phases were dried
- customevaporated to a pale buff solid (3.13 g)
- customThis was purified by CC
- washeluting with System A 1:1
출처 및 근거
- ORD 기록
- ord-40d4fd87b891429f97138470c0771931
- 출처 데이터셋
- uspto-grants-1992_06
- 특허 번호
- US05120848
연결된 노트
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