反应详情

In 63 ml of water was dissolved 6.93 g of glycine, and under ice-cooling, 15 g of 2-n-propyl-n-pentanoyl chloride and 13 ml of a 36% sodium hydroxide solution were alternately added dropwise. After completion of the dropwise addition, the mixture was stirred at room temperature for 3 hours to conduct the reaction, adjusted a pH thereof to about 2 with a 1 N hydrochloric acid, and precipitated crystals were collected by filtration. The crystals were dissolved in ethyl acetate, washed with a saturated saline solution and then dried over anhydrous magnesium sulfate. Crystals obtained by condensing the solvent under reduced pressure were recrystallized from hexane-ethyl acetate to give 10.9 g (Yield: 59%) of the title compound as colorless needle crystals.

1. temperatureunder ice-cooling
2. additionAfter completion of the dropwise addition
3. customthe reaction
4. customto about 2 with a 1 N hydrochloric acid, and precipitated crystals
5. filtrationwere collected by filtration
6. dissolutionThe crystals were dissolved in ethyl acetate
7. washwashed with a saturated saline solution
8. dry with materialdried over anhydrous magnesium sulfate
9. customCrystals obtained by condensing the solvent under reduced pressure
10. customwere recrystallized from hexane-ethyl acetate