反应详情

In this example, L-proline (11.5 g; 0.10 mole) and caustic soda (8.0 g; 0.2 moles) are dissolved in 100 ml water, and a solution of p-methylphenylsulfonyl chloride (20.9 g) dissolved in ether (80 ml) is added thereto with vigorous stirring under cooling in an ice bath (5°-10° C.). After reaction for about 5 hours, the reaction mixture is left standing, and the upper ether layer is removed. The remaining aqueous layer is admixed with 2N hydrochloric acid to adjust the pH to 3-4. After being left standing in a cool place (0°-5° C.), the deposited crystals are filtered off. The crystals are recrystallized from an aqueous 60% ethanol solution (about 200 ml), whereby p-methylphenylsulfonyl-L-proline (compound number 15; 20.1 g; m.p. 57°-59° C.) was obtained. Yield: 70%.

1. additionis added
2. temperatureunder cooling in an ice bath (5°-10° C.)
3. customAfter reaction for about 5 hours
4. waitthe reaction mixture is left
5. customthe upper ether layer is removed
6. waitAfter being left
7. customstanding in a cool place (0°-5° C.)
8. filtrationthe deposited crystals are filtered off
9. customThe crystals are recrystallized from an aqueous 60% ethanol solution (about 200 ml)