反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
12.3 g of 1,4-dihydroxy-2-naphthoic acid was dissolved in 100 ml of dimethylformamide, and to the solution was added 23.2 g of a 28% methanolic solution of sodium methylate in a nitrogenous atmosphere at 40° C. with stirring. The mixture was heated to 60° C., and 15.3 g of hexadecyl bromide was added thereto dropwise over a period of 30 minutes. The resulting mixture was heated for 3 hours while stirring, cooled, and then poured into 1 liter of ice-water to which 50 ml of concentrated hydrochloric acid had already been added with stirring. The precipitated crude crystals were filtered and washed with water. After addition of 1 g of activated carbon, the mixture was dissolved in 100 ml of methanol while heating. The activated carbon was filtered, and the filtrate was cooled. The precipitated crystals were filtered, washed with methanol and dried to obtain 9.4 g of 1-hydroxy-4-hexadecyloxy-2-naphthoic acid. Melting Point: 121°-124° C.
WORKUP
后处理
- temperatureThe resulting mixture was heated for 3 hours
- stirringwhile stirring
- temperaturecooled
- additionhad already been added
- stirringwith stirring
- customThe precipitated crude crystals
- filtrationwere filtered
- washwashed with water
- additionAfter addition of 1 g of activated carbon
- dissolutionthe mixture was dissolved in 100 ml of methanol
- temperaturewhile heating
- filtrationThe activated carbon was filtered
- temperaturethe filtrate was cooled
- filtrationThe precipitated crystals were filtered
- washwashed with methanol
- customdried