反应详情

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0 °C

9 g of fluorosulfonic acid was cooled to -78° C. with dry ice-acetone, 30 ml of 1-pentene was gradually dropwise added thereto under stirring. After completion of the dropwise addition, the stirring was continued at the same temperature for 15 minutes. 100 ml of methylene chloride which was previously cooled to -78° C., was added thereto, and then 15 g of 2-nitrobenzamide was added thereto at once. Then, the reaction was conducted for 12 hours under stirring while the temperature of the solution was returned to room temperature. After completion of the reaction, the reaction solution was poured into a mixture of 250 ml of a 1N sodium hydroxide aqueous solution and 100 ml of methylene chloride, which was cooled to 0° C., and then the mixture was vigorously stirred for 10 minutes. The reaction solution was extracted, and the extract was washed with water and then dried over Glauber's salt. After distillation of the solvent, the residue was purified by silica gel column chromatography to obtain 0.3 g of oily 1-methylbutyl 2-nitrobenzimidate (Intermediate Compound No. 63).

1. additionwas gradually dropwise added
2. additionAfter completion of the dropwise addition
3. additionwas added
4. waitThen, the reaction was conducted for 12 hours
5. stirringunder stirring while the temperature of the solution
6. customwas returned to room temperature
7. customAfter completion of the reaction
8. stirringthe mixture was vigorously stirred for 10 minutes
9. extractionThe reaction solution was extracted
10. washthe extract was washed with water
11. dry with materialdried over Glauber's salt
12. distillationAfter distillation of the solvent
13. customthe residue was purified by silica gel column chromatography