반응 #353004

반응 방정식

α-methylstyrene

2-(2,4-dihydroxyphenyl)-4,6-bis-(2,4-dimethylphenyl)-s-triazine

methyl styrene

→

title compound

수율 67.7%

2-[2,4-Dihydroxy-5-(1-methyl-1 -phenylethyl)phenyl]-4,6-bis-(2,4-dimethylphenyl)-s-triazine

수율 67.7%

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타To a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer, condenser
2. 2
   온도After cooling to room temperature
3. 3
   세척washed twice with water and once with brine
4. 4
   건조is dried over anhydrous magnesium sulfate
5. 5
   여과filtration
6. 6
   기타the solvent is removed under reduced pressure
7. 7
   기타to yield a yellow solid
8. 8
   기타The crude product is purified with medium pressure chromatography with 12% ethyl acetate/heptane

실험 절차

To a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer, condenser, dropping funnel, thermometer, and a nitrogen atmosphere are charged 15.0 g (37.8 mmol) of 2-(2,4-dihydroxyphenyl)-4,6-bis-(2,4-dimethylphenyl)-s-triazine and 390 mg of aluminum isopropoxide. The mixture is heated to 175° C. and 4.47 g (37.9 mmol) of α-methylstyrene are added dropwise at a rate of one drop every two seconds. A total of six equivalents of or-methyl styrene are added in this fashion over a 4.5 hour period. After cooling to room temperature, the mixture is diluted with ethyl acetate, washed twice with water and once with brine, and is dried over anhydrous magnesium sulfate. Following filtration, the solvent is removed under reduced pressure to yield a yellow solid. The crude product is purified with medium pressure chromatography with 12% ethyl acetate/heptane to afford 13.2 g of the title compound as a yellow solid; mp 168°-170° C.

출처