反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Research Disclosure, January 1975, 27, concerns incorporated dye-forming blocked developers. In accordance with the process disclosed, a mixture of 65.7 g (0.37 mole) of 2-morpholinomethyl-1-naphthol, 15 g of 10% Pd/C, and 540 ml of ethanol was hydrogenated at ambient temperature and at an initial pressure of 62 psi. The theoretical amount of hydrogen was absorbed in approximately one hour. The catalyst was removed by filtration and the filtrate was concentrated under vacuum. The residue was taken up in ether, extracted with 10% hydrochloric acid then with saturated aqueous NaCl, dried over anhydrous sodium sulfate, then concentrated under vacuum to yield 37.9 g 2-methyl-1-naphthol (65% yield). The acetate (1) was prepared in a yield of 61% using acetic anhydride-pyridine. The overall yield was 40%. This prior art process is disadvantageous in that the intermediate compound, 2-morpholinomethyl-1-naphthol, does not precipitate from water, thus an extraction step is required. Moreover, high loading (20%) of 10% Pd/C is required. Still further, both an extraction step and acetylation step are necessary. Thus, the entire process disadvantageously requires three steps.
WORKUP
后处理
- customResearch Disclosure, January 1975, 27, concerns incorporated dye-forming
- customwas hydrogenated at ambient temperature
- customThe theoretical amount of hydrogen was absorbed in approximately one hour
- customThe catalyst was removed by filtration
- concentrationthe filtrate was concentrated under vacuum
- extractionextracted with 10% hydrochloric acid
- dry with materialwith saturated aqueous NaCl, dried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum