反応 #42037

反応方程式

ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate

→

objective compound

収率 97.5%

ethyl 4-(1-methylpiperidin-4-ylmethyl)-3-trifluoromethylbenzoate

収率 97.5%

溶媒

methanol

反応条件

後処理

1. 1
   その他The catalyst was removed by filtration
2. 2
   workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
3. 3
   workup.DISSOLUTIONThe mixture was again dissolved in 32 ml of methanol
4. 4
   workup.ADDITION78 mg of 10% palladium-carbon was added
5. 5
   workup.WAITthe mixture was hydrogenated at room temperature under 1 atm for 4 hours
6. 6
   workup.ADDITIONFurther, 78 mg of palladium-carbon was added
7. 7
   workup.WAITthe mixture was hydrogenated at room temperature under 1 atm for 24 hours
8. 8
   workup.ADDITION78 mg of palladium-carbon was further added
9. 9
   workup.WAITthe mixture was hydrogenated at room temperature under 1 atm for 19 hours
10. 10
    その他The catalyst was removed by filtration
11. 11
    workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure

実験手順

1.57 g of ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate (Reference Example 7 (step 2)) was dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added, and then the mixture was hydrogenated at room temperature under 1 atm for 24 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure. The mixture was again dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added thereto, and then the mixture was hydrogenated at room temperature under 1 atm for 4 hours. Further, 78 mg of palladium-carbon was added and the mixture was hydrogenated at room temperature under 1 atm for 24 hours. 78 mg of palladium-carbon was further added and the mixture was hydrogenated at room temperature under 1 atm for 19 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure to obtain 1.54 g of the objective compound as a green oily product.

出典