反应详情

温度

145 °C

In a 100-ml eggplant-shaped flask were charged 2.68 g (20 mmol) of trimethylolpropane (manufactured by Tokyo Kasei Kogyo Co., Ltd.), 7.57 g (63 mmol) of 2-mercaptoisobutanoic acid, 0.23 g (1.2 mmol) of p-toluenesulfonic acidmonohydrate, and 20 g of toluene, and a Dean-Stark apparatus and a condenser tube were equipped thereto. While the contents being stirred, they were heated at an oil bath temperature of 145° C. After 3 hours from the start of the reaction, the reaction mixture was left to cool and neutralized with 50 ml of an aqueous 5% sodium hydrogen carbonate solution. Further, the reaction mixture was washed with deionized water two times, and then dehydrated and dried over anhydrous magnesium sulfate. Then, the toluene was distilled off and the residue was subjected to column chromatography with silica gel to purify TPMIB. The silica gel used was Wako Gel C-200, and n-hexane/ethyl acetate=5/1 (by volume ratio) was used as an elution solvent. The TPMIB obtained by the purification was a white crystal and the yield was 4.50 g (51%). The TPMIB had a compositional formula of Cl18H32O6S3 and a molecular weight of 440.64.

1. customa Dean-Stark apparatus and a condenser tube were equipped
2. customAfter 3 hours from the start of the reaction
3. waitthe reaction mixture was left
4. temperatureto cool
5. washFurther, the reaction mixture was washed with deionized water two times
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThen, the toluene was distilled off
8. customto purify TPMIB
9. customThe TPMIB obtained by the purification