反応 #652768

反応方程式

dimethyldodecylamine

chloromethylthiocyanate

→

Dimethyldodecyl(thiocyanatomethyl)ammonium Chloride

収率 79.4%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他A considerable amount of solids was formed
2. 2
   workup.STIRRINGThe reaction was then stirred for 7 more hours at 35° C
3. 3
   ろ過The solid was filtered off with suction
4. 4
   洗浄the solid washed with diethyl ether
5. 5
   その他The filtrate now formed more solid which
6. 6
   ろ過was filtered off
7. 7
   洗浄washed with ether
8. 8
   その他to air dry to constant weight, 331.0 g, for a 79.4% yield

実験手順

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%.

出典