Ammonium Hydroxide → 5-Chloropentanesulfonamide

2.5 ml of a 28% aqueous solution of ammonium hydroxide were added dropwise at 0° to +5° C. under an inert gas atmosphere to a solution of 2.5 g of 5-chloropentane sulfonyl chloride (preparation described in: Bull. Soc. Chim. Belg. (1965) Vol. 74., p. 21) in 30 ml of tetrahydrofuran. The temperature was allowed to rise from 3° C. to 16° C., and the mixture was stirred at ambient temperature for 2 hours. The tetrahydrofuran was evaporated under reduced pressure and the residue was taken up in water, extracted with methylene chloride, washed with water, then with an aqueous solution of sodium chloride, dried and evaporated under reduced pressure to obtain 2.01 g of the expected product melting at 62° C.

1. customto rise from 3° C. to 16° C.
2. customThe tetrahydrofuran was evaporated under reduced pressure
3. extractionextracted with methylene chloride
4. washwashed with water
5. dry with materialwith an aqueous solution of sodium chloride, dried
6. customevaporated under reduced pressure

ORD record

ord-c163d5683b9a4217b9fdabfcd2b0a7a9

Source dataset

uspto-grants-1996_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05494907