反应详情

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%.

1. customA considerable amount of solids was formed
2. stirringThe reaction was then stirred for 7 more hours at 35° C
3. filtrationThe solid was filtered off with suction
4. washthe solid washed with diethyl ether
5. customThe filtrate now formed more solid which
6. filtrationwas filtered off
7. washwashed with ether
8. customto air dry to constant weight, 331.0 g, for a 79.4% yield