反应详情

1.0 g of (E)-N-ethyl-6,6-dimethyl-2-hepten-4-ynylamine hydrochloride was dissolved in 20 ml of dimethylformamide, and 0.7 g of methyl bromoacetate and 1.0 g of potassium carbonate were added. The mixture was stirred overnight at room temperature, and worked up in a customary manner. The resulting glycine ester compound was dissolved in a methanol solution (50 ml) of 0.5 g of sodium hydroxide, and 25 ml of water was added. The mixture was stirred at room temperature for 2 hours, and the solvent was evaporated. The residue was dissolved in water, and the solution was made weakly acidic with hydrochloric acid, then butanol and a saturated aqueous solution of sodium chloride were added. The organic layer was separated and the solvent was evaporated, then the residue was dissolved in a 10% hydrogenchloridemethanol solution. The solvent was re-evaporated, and the residue was treated with hexane to give 1.36 g of the captioned compound as a pale yellow powder.

1. additionwas added
2. stirringThe mixture was stirred at room temperature for 2 hours
3. customthe solvent was evaporated
4. dissolutionThe residue was dissolved in water
5. additionbutanol and a saturated aqueous solution of sodium chloride were added
6. customThe organic layer was separated
7. customthe solvent was evaporated
8. dissolutionthe residue was dissolved in a 10% hydrogenchloridemethanol solution
9. customThe solvent was re-evaporated
10. additionthe residue was treated with hexane