反应详情

A mixture of acetamidine hydrochloride (28.8 g., 0.15 mole) and 50% sodium hydroxide (12.0 g., 0.15 mole) in 150 ml. of acetone is stirred for a period of 10 min. to liberate the free base. A solution of styrylsulfonyl chloride (10.1 g., 0.05 mole) in 50 ml. of acetone is added dropwise to the mixture at a temperature of 20°-25° C. with stirring. After further stirring for 10 min., the mixture is concentrated under reduced pressure to remove acetone, the concentrate diluted with 200 ml. of water and acidified with 3 N hydrochloric acid to provide a precipitate. The precipitate is collected, dissolved in chloroform and the chloroform extract dried. Evaporation of the chloroform solvent under reduced pressure provides a white solid, m.p. 130°-134° C. which is crystallized from isopropyl acetate affording 8.5 g. (76% yield) of N-(STYRYLSULFONYL)ACETAMIDINE, m.p. 134.5°-137.0° C. (corr.).

1. stirringAfter further stirring for 10 min.
2. concentrationthe mixture is concentrated under reduced pressure
3. customto remove acetone
4. additionthe concentrate diluted with 200 ml
5. customto provide a precipitate
6. customThe precipitate is collected
7. dissolutiondissolved in chloroform
8. extractionthe chloroform extract
9. customdried
10. customEvaporation of the chloroform solvent under reduced pressure
11. customprovides a white solid, m.p. 130°-134° C. which
12. customis crystallized from isopropyl acetate affording 8.5 g