تفاعل #1808467
ord-3635554a77c149f9b9b46b6e1e667db9
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىevaporated under reduced pressure
- 2أخرىthe residue partitioned between water and diethylether
- 3استخلاصThe ether extract
- 4تجفيفwas dried with sodium sulphate
- 5ترشيحfiltered
- 6أخرىevaporated
- 7workup.DISSOLUTIONThe residue was dissolved in the minimum of hot 1:1 dimethylether-hexane
- 8أخرىcrystallised
- 9درجة 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 diethylether. 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°.