反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Powdered anhydrous potassium carbonate (4.3 kg, 31 moles) was added to a mixture of 1,3-dibromopropane (6.55 kg, 32 moles), thiophenol (1.2 kg, 10.9 moles) and methylethylketone (9 L). The alkylation was carried out under a hood in a 22 liter flask equipped with a mechanical stirrer, heating mantle, and 2 reflux condensers. Nitrogen gas was passed over the top of the condensers. Within 30 minutes the mixture had generated enough heat to attain reflux. Reflux was then maintained for another 30 to 60 minutes. The mixture was permitted to come to room temperature over an 18 hour period. The solvent layer was siphoned off and filtered through celite. The salts were filtered and washed with acetone. The filtrates were concentrated. The residue was vacuum distilled. Three fractions were collected:
WORKUP
后处理
- customThe alkylation was carried out under a hood in a 22 liter flask
- customequipped with a mechanical stirrer
- temperatureheating mantle
- temperature2 reflux condensers
- temperatureWithin 30 minutes the mixture had generated enough heat
- temperatureto attain reflux
- temperatureReflux
- temperaturewas then maintained for another 30 to 60 minutes
- filtrationfiltered through celite
- filtrationThe salts were filtered
- washwashed with acetone
- concentrationThe filtrates were concentrated
- distillationdistilled
- customThree fractions were collected