反应详情

A 250 ml tri-neck round bottom flask was equipped and a 50 ml addition funnel and the flask was cooled <0 C. 30 g of 1-methylcyclopentanol (0.3 M, 1 EQ) was added to the flask. 70% H2SO4 solution was prepared and cooled in an ice bath. The H2SO4 (12.71 ml, 0.91 M, 3 EQ) was added drop wise over 15 minutes and the reaction mixture was stirred for ˜2.5 hours in order to allow all the 1-methylcyclopentanol to dissolve. With the reaction stirring, 8.11 ml of H2O2 35% (wt) (0.24 M, 0.8 EQ) was added drop wise over 15 minutes. The reaction was left stirring overnight. The reaction mixture was transferred to a separation funnel and extracted three times with 50 ml of pentane each time. Organic layers were collected and the aqueous was set aside. The organic layers were extracted 3 times with 50 ml of 1N NaOH each time to remove excess acid. The organic layer was collected, dried and concentrated. The residue was purified by chromatography on a silica column using pentane as the mobile phase. The product fractions were concentrated to yield 973 mg of di(1-methyl-cyclopentyl)peroxide as a colorless oil. 13C-NMR (CDCl3) δ 24.43, 24.75, 37.13, 89.23

1. customA 250 ml tri-neck round bottom flask was equipped
2. additiona 50 ml addition funnel
3. temperaturethe flask was cooled <0 C
4. temperaturecooled in an ice bath
5. dissolutionto dissolve
6. stirringWith the reaction stirring
7. waitThe reaction was left
8. stirringstirring overnight
9. customThe reaction mixture was transferred to a separation funnel
10. extractionextracted three times with 50 ml of pentane each time
11. customOrganic layers were collected
12. extractionThe organic layers were extracted 3 times with 50 ml of 1N NaOH each time
13. customto remove excess acid
14. customThe organic layer was collected
15. customdried
16. concentrationconcentrated
17. customThe residue was purified by chromatography on a silica column
18. concentrationThe product fractions were concentrated