Reaktionsgleichung
[F:1][C:2]([F:13])([F:12])[S:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10]N)=[CH:6][CH:5]=1.[CH3:14][CH:15]([C:24](=O)[CH3:25])[CH2:16][CH2:17][CH2:18][CH2:19][S:20]([OH:23])(=[O:22])=[O:21]>C(O)(=O)C>[F:1][C:2]([F:13])([F:12])[S:3][C:4]1[CH:9]=[C:8]2[C:7](=[CH:6][CH:5]=1)[N:10]=[C:24]([CH3:25])[C:15]2([CH3:14])[CH2:16][CH2:17][CH2:18][CH2:19][S:20]([OH:23])(=[O:21])=[O:22]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To 4-(trifluoromethylthio)phenylhydrazine (1 g) in acetic acid (40 ml) was added 5-methyl-6-oxoheptane-1-sulphonic acid (1.4 g) and the solution heated to reflux overnight. The volatiles were removed on a rotary evaporator to give the crude product, 1.1 g of which was purified by preparative HPLC. The relevant fractions were combined, concentrated on a rotary evaporator and freeze dried to give the desired product (260 mg). M+=381
Aufarbeitung
- temperaturethe solution heated
- temperatureto reflux overnight
- customThe volatiles were removed on a rotary evaporator
- customto give the crude product, 1.1 g of which
- customwas purified by preparative HPLC
- concentrationconcentrated on a rotary evaporator and freeze
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-7773518b75a34179bcb983a4bc6863e6
- Quelldatensatz
- uspto-grants-2010_08
- Patentnummer
- US07767829B2
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