Thionyl Chloride → 1003-85-6

Temperature

40 °C

104.15 g of 2.2-dimethyl-1,3-propanediol (1 mol) are suspended in 200 ml of methylene chloride in a 500 ml four-necked flask which is provided with a stirrer, a reflux condenser, a thermometer and a dropping funnel. 125 g (1.05 mol) of thionyl chloride are added dropwise within 1 hour while stirring at 5°-10° C. The reaction mixture is then warmed to 40° C. for 3 hours. The thusobtained oil is washed with 50 ml of water and then with 50 ml of NaHCO3 solution and dried over Na2SO4. After removing the majority of methylene chloride on a rotary evaporator the residue is distilled at 85°-87° C./30 mmHg over a 10 cm isolated column filled with Raschig rings. There are obtained 142.5 g of 5,5-dimethyl-1,3,2-dioxathiane 2-oxide in the form of a colourless oil.

1. customwhich is provided with a stirrer, a reflux condenser
2. washThe thusobtained oil is washed with 50 ml of water
3. dry with materialwith 50 ml of NaHCO3 solution and dried over Na2SO4
4. customAfter removing the majority of methylene chloride
5. customon a rotary evaporator the residue
6. distillationis distilled at 85°-87° C./30 mmHg over a 10 cm
7. customisolated column
8. additionfilled with Raschig rings

ORD record

ord-2e5a0675196445c08f464c545438b81f

Source dataset

uspto-grants-1986_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04596879