Reaktion #652768
ord-eb7a11205d7645a18d93c723d47218df
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeA considerable amount of solids was formed
- 2workup.STIRRINGThe reaction was then stirred for 7 more hours at 35° C
- 3FiltrationThe solid was filtered off with suction
- 4Waschenthe solid washed with diethyl ether
- 5SonstigeThe filtrate now formed more solid which
- 6Filtrationwas filtered off
- 7Waschenwashed with ether
- 8Sonstigeto air dry to constant weight, 331.0 g, for a 79.4% yield
Vorschrift
A 2 liter flask was charged with 1 liter of tetrahydrofuran, 277 g of dimethyldodecylamine and then 153.7 g of chloromethylthiocyanate. The reaction mixture was stirred at ambient temperature for 17 hours. A considerable amount of solids was formed. The reaction was then stirred for 7 more hours at 35° C. The solid was filtered off with suction and the solid washed with diethyl ether. The filtrate now formed more solid which was filtered off, washed with ether and then combined with the other solid. The combined solids were now allowed to air dry to constant weight, 331.0 g, for a 79.4% yield. Analysis (nmr) showed a purity of better than 98%.