تفاعل #1869177

ord-47698fe631f744f7bb78fc6f4bd9c905

معادلة التفاعل

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
المردود 100.3%
O=C1CCN(C(=O)OCc2ccccc2)CC1
N-benzyloxycarbonyl-4-piperidone
المردود 100.3%

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe aqueous solution was extracted three times with ethyl acetate
  2. 2
    غسيلThe organic layer was washed with a saturated aqueous solution of sodium bicarbonate
  3. 3
    تجفيفa saturated aqueous solution of sodium chloride subsequently, dried over anhydrous magnesium sulfate
  4. 4
    تركيزconcentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07498323B2uspto-grants-2009_03