Sulfuric Acid → HCID 20135952, compound

Temperature

25 °C

To 253 g. (0.85 mol) of perfluoro-(N-methyl-morpholine) in a 300 ml. autoclave is added 72 g. (0.9 mol) of sulfur trioxide. The vessel is sealed, heated and rocked at 120° C. for 6 hrs. The autoclave is then cooled to 25° C., vented to release volatile materials and the residue charged to a 500 cc. flask equipped with magnetic stirrer, dropping funnel, condenser and thermometer. A solution of 195 g. of 96% sulfuric acid and 5 g. of H2C is added dropwise with stirring. The temperature is kept below 50° C. After the sulfuric acid is added the mixture is heated and stirred at reflux (55°-60° C.) for four hours. Distillation yields a large fraction, 207 g., b.p. 48°-65° C./740 mm., which consists of 45% by weight perfluoror-N-methyl-3-oxo-morpholine (40% conversion) and 15% by weight of higher boiling products believed to include perfluoro-(N-methyl-3,5dioxo-morpholine). Isolation of the pure amide (b.p. 59°-60° C./740 mm.) can be accomplished by distillation through a 25-plate column.

1. additionautoclave is added 72 g
2. customThe vessel is sealed
3. temperatureheated
4. additionthe residue charged to a 500 cc
5. customflask equipped with magnetic stirrer
6. additionof H2C is added dropwise
7. customis kept below 50° C
8. temperatureis heated
9. stirringstirred
10. temperatureat reflux (55°-60° C.) for four hours
11. distillationDistillation
12. customyields a large fraction, 207 g
13. distillationIsolation of the pure amide (b.p. 59°-60° C./740 mm.) can be accomplished by distillation through a 25-plate column

ORD record

ord-03ade2d2fb9449298dc0d305f78ccb4a

Source dataset

uspto-grants-1978_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04084050