Reaktionsgleichung
Br[CH2:2][CH2:3][C:4]1[CH:23]=[CH:22][C:7]([C:8]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[O:9])=[CH:6][CH:5]=1.N12CCCN=C1CCCCC2.Cl>C1COCC1>[CH:3]([C:4]1[CH:23]=[CH:22][C:7]([C:8]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[O:9])=[CH:6][CH:5]=1)=[CH2:2]Komponenten
5
Versuchsvorschrift
A solution of 35.85 g (0.09 mol) of N-[4-(2-bromoethyl)benzoyl]-4-methoxybenzenesulfonamide, 27.40 g (0.18 mol) of 1,8-diazabicyclo-[5.4.0]undec-7-ene (DBU) and 375 ml of THF was stirred at room temperature for 19.5 hrs. Solid formed within 30 mins. The mixture was poured into dilute HCl giving an oily precipitate which crystallized. The solid was collected, washed with water, redissolved in methylene chloride, dried over magnesium sulfate and concentrated to an oil which crystallized. The solid was collected, recrystallized from toluene, collected, washed with ligroine and dried.
Aufarbeitung
- customSolid formed within 30 mins
- customcrystallized
- customThe solid was collected
- washwashed with water
- dissolutionredissolved in methylene chloride
- dry with materialdried over magnesium sulfate
- concentrationconcentrated to an oil which
- customcrystallized
- customThe solid was collected
- customrecrystallized from toluene
- customcollected
- washwashed with ligroine
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-cbd759d9c45c482fbeab048a3d68cc39
- Quelldatensatz
- uspto-grants-1999_02
- Patentnummer
- US05874194
Verknüpfte Notizen
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