4,5-DIMETHYLBENZENE-1,2-DIMETHANOL synthesis
- Product Name:4,5-DIMETHYLBENZENE-1,2-DIMETHANOL
- CAS Number:60070-05-5
- Molecular formula:C10H14O2
- Molecular Weight:166.22
17649-59-1
19 suppliers
inquiry
60070-05-5
49 suppliers
$512.00/25g
Yield:60070-05-5 100%
Reaction Conditions:
Stage #1: dimethyl 4,5-dimethylphthalatewith lithium aluminium tetrahydride in tetrahydrofuran at -78 - 20;Reflux;
Stage #2: with phosphorus tribromide
Steps:
3
Preparation of 1,2-bis(bromomethyl)-4,5-dimethylbenzene Dried tetrahydrofurane (20 mL) was put into LAH (0.54 g, 14.29 mmol) at -78° C. Dimethyl 4,5-dimethylbenzene-1,2-dicarboxylate (1.27 g, 5.71 mmol) was dissolved in dried tetrahydrofurane (10 mL), and then the resultant mixture was slowly added into the above reaction solution. Then the reaction temperature was slowly raised to room temperature, and then stirring under reflux was performed for 24 hours. After the reaction, the resultant reaction material was cooled by a sodium hydroxide solution, and then concentrated under reduced pressure, followed by washing with ethyl acetate twice and again washing with distilled water once. The organic layer was separated, and dried over sodium sulfate, and then the solvent was concentrated under reduced pressure, thereby obtaining white solids, (4,5-dimethyl-1,2-phenylene)dimethanol (0.95 g, quantitative). This is subjected to a bromination reaction using tribromophosphine, thereby obtaining 1,2-bis(bromomethyl)-4,5-dimethyl benzene at a yield of 56%. 1H-NMR 300 MHz (CDCl3) δ 7.13 (s, 2H), 4.27 (s, 4H), 2.23 (s, 6H).
References:
US2012/4476,2012,A1 Location in patent:Page/Page column 9
5999-20-2
17 suppliers
$45.00/10mg
60070-05-5
49 suppliers
$512.00/25g
5680-10-4
24 suppliers
$97500.00/5G
60070-05-5
49 suppliers
$512.00/25g
69094-40-2
0 suppliers
inquiry
60070-05-5
49 suppliers
$512.00/25g
95-47-6
609 suppliers
$10.00/25g
60070-05-5
49 suppliers
$512.00/25g