تفاعل #94616

معادلة التفاعل

Triethylamine

phosgene

N-methylpentylamine

→

N-methyl-N-pentylcarbamoyl chloride

المذيبات

methylcyclohexane

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwhilst maintaining the temperature at -10° C
2. 2
   ترشيحThe insoluble material is then filtered off
3. 3
   غسيلwashed with toluene (80 cc.)
4. 4
   تجفيفThe organic solutions are dried over calcium chloride (10 g.)
5. 5
   ترشيحAfter filtration
6. 6
   أخرىthe solvents are evaporated under reduced pressure (40 mm.Hg)
7. 7
   workup.DISTILLATIONThe residue is distilled under reduced pressure

الإجراء التجريبي

Triethylamine (14 cc.) is added over the course of 8 minutes to a 2.5N solution (42 cc.) of phosgene in methylcyclohexane, cooled to -10° C., and a solution of N-methylpentylamine (13.7 cc.) in toluene (50 cc.) is then added whilst maintaining the temperature at -10° C. The mixture is stirred for 1 hour at +5° C. The insoluble material is then filtered off and washed with toluene (80 cc.). The organic solutions are dried over calcium chloride (10 g.). After filtration, the solvents are evaporated under reduced pressure (40 mm.Hg). The residue is distilled under reduced pressure to give N-methyl-N-pentylcarbamoyl chloride (5.6 g.), b.p. 120-125° C./40 mm.Hg.

المصدر