Diethyl Ether → HCID 18408917, compound

Temperature

0 °C

To a solution of 1 g of 4-oxopiperidine hydrochloride monohydrate in 0.7 ml of water was added 2.2 ml of diethyl ether, and the mixture was stirred at 0° C. Chloromethyl chloroformate (0.3 ml) was added dropwise, and the mixture was stirred at 0° C. for 5 minutes. Next, 0.8 ml of a 17N aqueous sodium hydroxide solution and 0.3 ml of chloromethyl chloroformate were divided into three portions and alternately added dropwise, and the resulting mixture was stirred at 0° C. for additional 20 minutes. The reaction mixture was diluted with 5 ml of a saturated aqueous saline, and extracted three times with 5 ml of diethyl ether. The organic layer thus obtained was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure to give 1.7 g (100%) of 1-chloromethoxycarbonyl-4-oxopiperidine.

1. stirringthe mixture was stirred at 0° C. for 5 minutes
2. additionalternately added dropwise
3. stirringthe resulting mixture was stirred at 0° C. for additional 20 minutes
4. additionThe reaction mixture was diluted with 5 ml of a saturated aqueous saline
5. extractionextracted three times with 5 ml of diethyl ether
6. customThe organic layer thus obtained
7. dry with materialwas dried over anhydrous sodium sulfate
8. customthe solvent was removed by distillation under reduced pressure

ORD record

ord-b47f91759326420283606569938243f6

Source dataset

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06472397B1