Reaktionsgleichung
C[Al](C)C.CC([SH:8])C.[Al].[CH3:10][O:11][C:12]1[N:17]=[C:16]([CH3:18])[N:15]=[C:14]([NH:19][C:20]([NH:22][S:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[C:32](OC)=O)(=[O:25])=[O:24])=[O:21])[N:13]=1.Cl.[C:37]1([CH3:43])C=CC=C[CH:38]=1>>[CH3:10][O:11][C:12]1[N:17]=[C:16]([CH3:18])[N:15]=[C:14]([NH:19][C:20]([NH:22][S:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[C:32]([CH:37]([CH3:43])[CH3:38])=[S:8])(=[O:24])=[O:25])=[O:21])[N:13]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
To 1.5 ml (2N) trimethylaluminum in 5 ml dry toluene under N2 was added dropwise 0.48 g (6.0 mmole) 2-propanethiol in 2 ml toluene. The resultant aluminum reagent was stirred at room temperature for 15 minutes, and 0.95 g (2.5 mmole) N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide was added in one portion. The suspension was heated to 80° C. for 3 hours, cooled to room temperature and 10% HCl (15 ml) was added. The mixture was stirred until a fine solid precipitated which was filtered off, washed with hexanes and air dried to yield 0.4 g of product melting at 155°-158° C. It showed infrared absorption peaks consistent for N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2-isopropylthiocarbonylbenzenesulfonamide.
Aufarbeitung
- temperaturecooled to room temperature
- customprecipitated which
- filtrationwas filtered off
- washwashed with hexanes and air
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-47aeae41c9144de292fb97a14d207867
- Quelldatensatz
- uspto-grants-1985_10
- Patentnummer
- US04545808
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