Phosphorus pentachloride → 3-Azidopropane-1-sulfonyl chloride

3-Azidopropanesulfonic acid, sodium salt 5 (1.87 g, 10.0 mmol) was suspended in dry benzene (20 mL), and PCl5 (2.3 g, 10.5 mmol) was added to the suspension. The mixture was stirred at room temperature for 30 minutes, then at gentle reflux for about 1 hour. The benzene and P(O)C13 were removed by evaporation under reduced pressure. Benzene was added to the crude mixture and the solvent was removed again under reduced pressure. The residue was dried in vacuo. The dried residue was dissolved in dichloromethane (anhydrous, 15 mL) and cooled at −10° C. using an ice/acetone bath.

1. temperatureat gentle reflux for about 1 hour
2. customThe benzene and P(O)C13 were removed by evaporation under reduced pressure
3. additionBenzene was added to the crude mixture
4. customthe solvent was removed again under reduced pressure
5. customThe residue was dried in vacuo
6. dissolutionThe dried residue was dissolved in dichloromethane (anhydrous, 15 mL)
7. temperaturecooled at −10° C.

ORD record

ord-65a36dd429d647bda6e8561d8289c1a2

Source dataset

uspto-grants-2008_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07414076B2