반응 #1869177

ord-47698fe631f744f7bb78fc6f4bd9c905

반응 방정식

Cl.O.O=C1CCNCC1
4-piperidone hydrochloride monohydrate
O=C(Cl)OCc1ccccc1
benzyloxycarbonyl chloride
Cl
hydrochloric acid
O=C1CCN(C(=O)OCc2ccccc2)CC1
title compound
수율 100.3%
O=C1CCN(C(=O)OCc2ccccc2)CC1
N-benzyloxycarbonyl-4-piperidone
수율 100.3%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the aqueous solution was extracted three times with ethyl acetate
  2. 2
    세척The organic layer was washed with a saturated aqueous solution of sodium bicarbonate
  3. 3
    건조a saturated aqueous solution of sodium chloride subsequently, dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated

실험 절차

A 4-piperidone hydrochloride monohydrate (15.3 g) was dissolved in 2N aqueous solution of sodium hydroxide (100 mL). To the solution was added a benzyloxycarbonyl chloride (20.4 g) at 0° C. The mixture was stirred for 1 hour. The reaction mixture was neutralized with 2N hydrochloric acid, and the aqueous solution was extracted three times with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride subsequently, dried over anhydrous magnesium sulfate and concentrated to give the title compound (23.3 g) having the following physical data.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07498323B2uspto-grants-2009_03