DI-M-TOLYL CARBONATE synthesis
- Product Name:DI-M-TOLYL CARBONATE
- CAS Number:620-52-0
- Molecular formula:C15H14O3
- Molecular Weight:242.27
Yield:620-52-0 95%
Reaction Conditions:
Stage #1: 3-methyl-phenolwith sodium hydroxide in water at 10; for 0.5 h;
Stage #2: bis(trichloromethyl) carbonatewith triethylamine in dichloromethane;water at 10 - 40; pH=9; for 2 h;Reagent/catalyst;Solvent;
Steps:
1; 2 Example 1
Put 46 grams of sodium hydroxide into a 250ml three-necked flask in turn, add 280 grams of water to dissolve it, cool to 10°C, slowly add 108 grams of m-cresol, stir for half an hour until all the reactants are dissolved, add 1 gram of triethylamine, adjust the pH When the value reaches 9, dissolve 51 grams of triphosgene in 250 grams of dichloromethane and slowly add dropwise to the above mixture. The addition is completed in 1 hour. After the dripping, the temperature is raised to 40°C and refluxed for 1 hour. After cooling to room temperature, the organic phase is separated , The organic phase was washed with dilute hydrochloric acid and pure water to neutrality, dried over anhydrous magnesium sulfate, distilled off the dichloromethane, and then crystallized and dried with 90% ethanol water to obtain 115 g of the product with a yield of 95%.
References:
CN108046998,2020,B Location in patent:Paragraph 0035-0038
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