反应详情

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. customdried
6. customevaporated under reduced pressure