1-METHALLYL-2-(2-HYDROXY-5-METHYL PHENYL) BENZOTRIAZOLE synthesis
- Product Name:1-METHALLYL-2-(2-HYDROXY-5-METHYL PHENYL) BENZOTRIAZOLE
- CAS Number:98809-58-6
- Molecular formula:C17H17N3O
- Molecular Weight:279.34
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98809-58-6
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Yield: 86%
Reaction Conditions:
with N,N-dimethyl-aniline;triethylamine in butanone at 80 - 180;Product distribution / selectivity;Inert atmosphere;Molecular sieve;Claisen rearrangement;
Steps:
3
EXAMPLE 3Reaction with 4 Molecular Sieve10 g of 2-(2-hydroxy-5-methylphenyl) benzotriazole (0.044 moles), 4.5 g of the triethylamine (0.044 moles), 16.1 g of N,N-dimethylaniline (0.13 moles) and 16 g of 4 molecular sieves (that are UOP type 4 beads purchased from the Fluka company) were introduced into the reacting chamber and mixed to form a solution. 0.09 moles of 3-chloro-2-alkyl propylene was dissolved in methyl ethyl ketone and added to the solution within 10 minutes into the reacting chamber where air in the reacting chamber was nitrogen. Then, the solution was heated to 80° C. for 5 hours and a reaction completion was monitored using HPLC. Then, the solution was heated to 180° C. and held on for 3 hours to allow Claisen rearrangement and left to cool to 80° C. Then, the solution was filtered using active carbon. A filtrate was recrystallized using 40 ml of isopropanol. Then, filter paper was used to filter a white recrystallized filtrate being 10.7 g of 1-methallyl-2-(2'-hydroxyl-5'-methylphenyl) benzotriazole (yield: 86%, purity: 99.9%, melting point: 95° C.).
References:
Lu, Ling;Wei, Po-Hsuan;Fan, Chung-Ning;Lee, Yu-Cheng;Yang, Hui-Ling;Lee, Yu-Chin US2009/270632, 2009, A1 Location in patent:Page/Page column 2; 3
2440-22-4
461 suppliers
$8.00/25g
563-47-3
253 suppliers
$10.00/5g
![[(2-methyl-2-propenyl)oxy]phenyl]-](/CAS/20180808/GIF/2170-60-7.gif)
2170-60-7
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98809-58-6
64 suppliers
$160.00/500mg
2170-60-7
2 suppliers
inquiry
98809-58-6
64 suppliers
$160.00/500mg