- Language
- 🇺🇸
- Joined
- Aug 10, 2023
- Messages
- 43
- Reaction score
- 8
- Points
- 8
1.4 kg of cyclohexylmethanol, 8.4 L of toluene and 969.8 g of pyridine were added to a 20 L four-neck flask, the system was cooled to 0 to 10° C., then a mixture of 1.66 kg of phosphorus tribromide and 7 L of toluene was dropwise added, the temperature was controlled below 5° C. The dropwise addition was finished in about 1 h, the temperature was increased to room temperature and reacted for 10 h. Then the temperature was cooled to below 20° C., about 2.5 L of a sodium hydroxide solution having a concentration of 5% was dropwise added, then 1.85 kg of solid sodium hydroxide was added to form a mixture. Liquid separation was performed for the mixture, an obtained water phase was extracted twice with 4 L of toluene, organic phases obtained after the extraction were combined and washed with saturated salt water, the washed organic phases was dried with anhydrous sodium sulfate and then concentrated to obtain 1.73 kg of a crude product, reduced pressure distillation was performed to obtain 722.8 g yield of 33.3%.