تفاعل #71755

معادلة التفاعل

Ethyl acetate

Example ( 1e )

tert-Butyl cis(±)-4-amino-3-methoxypiperidine-1-carboxylate

sodium carbonate

benzyl chloroformate

→

title compound

المردود 90.6%

tert-Butyl cis(±)-4-{[(benzyloxy)carbonyl]amino}-3-methoxypiperidine-1-carboxylate

المردود 90.6%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   غسيلthe organic layer was washed with brine
2. 2
   تجفيفdried over anhydrous sodium sulfate
3. 3
   تركيزconcentration under reduced pressure
4. 4
   أخرىthe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=90/10, 50/50)

الإجراء التجريبي

tert-Butyl cis(±)-4-amino-3-methoxypiperidine-1-carboxylate obtained by the method described in Example (1e) (3.0 g, 13.0 mmol) was dissolved in THF (60 mL), followed by cooling to 0° C. Thereafter, aqueous sodium carbonate solution (30 mL) and benzyl chloroformate (2.8 mL, 19.6 mmol) were added, and the mixture was stirred for one hour. Ethyl acetate was added to the reaction solution, and the organic layer was washed with brine and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=90/10, 50/50) to obtain 4.29 g of the title compound as a pale yellow solid (90%).

المصدر