反应详情

In a mixture of 10 ml of water and 20 ml of ethyl acetate, 1.6 g of tyrosinol was dissolved. To the solution were added dropwise 2 g of 2-methylbenzyloxycarbonyl chloride and 10 ml of an aqueous solution containing 1.3 g of sodium carbonate alternately with stirring while cooling with ice. After stirring for two hours at room temperature, the ethyl acetate layer was collected and washed with 5% hydrochloric acid and then with water. The layer was dried and concentrated to dryness. The residue was crystallized from ethyl acetate-petroleum ether to give 2.2 g of N-(2-methylbenzyloxycarbonyl)-tyrosinol with a mp. 78°-81° C. in a yield of 70%. Analysis, calculated for C18H21O4N: C, 68.55; H, 6.72; N, 4.44; found C, 68.88; H, 6.84; N, 4.42.

1. dissolutionwas dissolved
2. temperaturewhile cooling with ice
3. stirringAfter stirring for two hours at room temperature
4. customthe ethyl acetate layer was collected
5. washwashed with 5% hydrochloric acid
6. customThe layer was dried
7. concentrationconcentrated to dryness
8. customThe residue was crystallized from ethyl acetate-petroleum ether