反応 #7309

反応方程式

4-methylpiperdine

triethylamine

methylchloroformate

water

→

product

4-Methyl-piperidine-1-carboxylic acid methyl ester

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   温度the mixture was cooled in an ice bath
2. 2
   その他the layers were separated
3. 3
   洗浄The organic layer was washed with dilute HCl
4. 4
   乾燥NaHCO3, and brine, and then the organic layer was dried over sodium sulfate
5. 5
   その他the solvent was removed in vacuo
6. 6
   workup.DISTILLATIONThe product was distilled at 90-93 C at ˜10 mm pressure

実験手順

To a three neck round bottom flask was added 360 g of 4-methylpiperdine, 470 mL of triethylamine, and 390 mL of methylene chloride and the mixture was cooled in an ice bath. To this mixture was added methylchloroformate (260 mL) in methylene chloride (215 mL) slowly to maintain a reaction temperature of 20 C or below. The reaction was stirred overnight, then 200 mL of water was added and the layers were separated. The organic layer was washed with dilute HCl, satd. NaHCO3, and brine, and then the organic layer was dried over sodium sulfate and the solvent was removed in vacuo. The product was distilled at 90-93 C at ˜10 mm pressure to provide 338 g of product.

出典