Chlorosulfonic acid → 2-Butyl-2-ethylaziridine

Acetonitrile (150 ml) and the product from (e) (20.0 g) were mixed under nitrogen, cooled to 2°-30° C. and chlorosulphonic acid (16.04 g, Aldrich) was added dropwise keeping the temperature below 10° C. The coolant was removed and the slurry left to stir for 80 minutes at room temperature. The reaction was concentrated in vacuo and co-distilled with water (50 ml). 50% Aqueous sodium hydroxide (55.2 g) and water (50 ml) were added and the mixture was distilled at atmospheric pressure. The organic layer was collected from the distillate and dried with solid potassium hydroxide to give the desired product (12.8 g). 1H NMR consistent with proposed structure.

1. temperaturecooled to 2°-30° C.
2. customthe temperature below 10° C
3. customThe coolant was removed
4. waitthe slurry left
5. concentrationThe reaction was concentrated in vacuo and co-distilled with water (50 ml)
6. addition50% Aqueous sodium hydroxide (55.2 g) and water (50 ml) were added
7. distillationthe mixture was distilled at atmospheric pressure
8. distillationThe organic layer was collected from the distillate
9. dry with materialdried with solid potassium hydroxide

ORD record

ord-f6a6a3ea17c34990ad46018e88f4db4e

Source dataset

uspto-grants-1997_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05663165