تفاعل #1816449

معادلة التفاعل

thiophosgene

DL-2-amino-1-hexanol

triethylamine

→

4-butyloxazolidine-2-thione

المذيبات

THF

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىevaporated under reduced pressure
2. 2
   أخرىthe residue partitioned between water and diethyl ether
3. 3
   استخلاصThe ether extract
4. 4
   تجفيفwas dried with sodium sulphate
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   workup.DISSOLUTIONThe residue was dissolved in the minimum of hot 1:1 dimethylether-hexane
8. 8
   أخرىcrystallised
9. 9
   درجة الحرارةon cooling

الإجراء التجريبي

To a stirred cold solution of DL-2-amino-1-hexanol (1.1 ml) in dry THF (10 ml) was added triethylamine (2.8 ml) followed by dropwise addition of thiophosgene (0.81 ml) in dry THF (9 ml). The mixture was then stirred for 18 h at 20° C., evaporated under reduced pressure and the residue partitioned between water and diethyl ether. The ether extract was dried with sodium sulphate filtered and evaporated. The residue was dissolved in the minimum of hot 1:1 dimethylether-hexane and crystallised on cooling to give 4-butyloxazolidine-2-thione, mp 71-2°.

المصدر