Reaktionsgleichung
[CH2:1]([O:3][C:4]1[C:9]([C:10](=[O:13])[NH:11][CH3:12])=[CH:8][N:7]=[C:6]([CH2:14][NH:15][C:16]([NH:18][C:19]([O:21][CH2:22][CH:23]2[C:35]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[C:29]3[C:24]2=[CH:25][CH:26]=[CH:27][CH:28]=3)=[O:20])=S)[CH:5]=1)[CH3:2]>O1CCOCC1.FC(F)(F)C([O-])=O.[Hg+2].FC(F)(F)C([O-])=O>[CH2:1]([O:3][C:4]1[C:9]([C:10](=[O:13])[NH:11][CH3:12])=[CH:8][N:7]2[C:16](=[N:18][C:19](=[O:20])[O:21][CH2:22][CH:23]3[C:35]4[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=4[C:29]4[C:24]3=[CH:25][CH:26]=[CH:27][CH:28]=4)[NH:15][CH:14]=[C:6]2[CH:5]=1)[CH3:2]Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
875 mg of N-(4-ethoxy-5-methylcarbamoyl pyridin-2-ylmethyl)-N′-(fluoren-9-ylmethyloxycarbonyl)thiourea (Example 19a, crude product) were dissolved in 25 ml of dioxane and treated at RT with 837 mg (1.96 mmol) of mercury(II) trifluoroacetate. After 10 minutes, the mixture was concentrated and the residue was taken up in DCM. The organic phase was washed three times with 4% strength LiCl solution and once with water, dried with MgSO4 and concentrated in a rotary evaporator. The crude product thus obtained (590 mg) was reacted further without further purification.
Aufarbeitung
- concentrationthe mixture was concentrated
- washThe organic phase was washed three times with 4% strength LiCl solution
- dry with materialonce with water, dried with MgSO4
- concentrationconcentrated in a rotary evaporator
Quellen und Nachweise
- ORD-Eintrag
- ord-8b381985904d458e8891b45a0d720ba1
- Quelldatensatz
- uspto-grants-2011_01
- Patentnummer
- US07863269B2
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