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
PROCEDURE
实验过程
To 17.0 g (0.05 mol) of the resulting 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-s-triazine were added 94.8 g (0.75 mol) of 2-bromoethanol and 85 g of dimethylformamide, and 29.2 g (0.35 mol) of a 48% aqueous solution of sodium hydroxide was added thereto dropwise at 85° C. The mixture was allowed to react at 85° C. for 10 hours, followed by cooling. The reaction mixture was neutralized with concentrated hydrochloric acid, and the precipitate was collected by filtration, washed with water, and dried to give 15.4 g (80%) of 2-hydroxy-4-(2-hydroxyethyloxy)phenyl-4,6-diphenyl-s-triazine (hereinafter referred to as HETr). To 15 g (0.039 mol) of the resulting HETr were added 6.8 g (0.047 mol) of octylic acid, 45 g of xylene, and 0.6 g of p-toluenesulfonic acid, and the mixture was heated under reflux at 140° C. for 10 hours. The reaction mixture was washed with water and recrystallized from a 1:3 mixed solvent of xylene and methanol to give 16.9 g (85%) of a pale yellow solid having a melting point of 109° C.
WORKUP
后处理
- additionwas added
- customdropwise at 85° C
- customto react at 85° C. for 10 hours
- temperatureby cooling
- filtrationthe precipitate was collected by filtration
- washwashed with water
- customdried