تفاعل #2555

ord-0679f3c83e8041a093c3b3901f299d06

معادلة التفاعل

Cl.O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
title compound
المردود 92.3%
O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine
المردود 92.3%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةWith cooling in an ice bath
  2. 2
    استخلاصThe reaction solution was extracted with ether
  3. 3
    غسيلwashed with saturated brine
  4. 4
    تجفيفthe resulting organic layer was dried on anhydrous sodium carbonate
  5. 5
    ترشيحThereafter, the organic layer was filtered through silica gel (5 g)
  6. 6
    أخرىthe solvent was removed by evaporation
  7. 7
    أخرىthe resulting residue was purified

الإجراء التجريبي

1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride (800 mg, 2.61 mmol) was suspended in ether (20 ml). With cooling in an ice bath, saturated sodium carbonate aqueous solution (5 ml) was added dropwise to the suspension. The reaction solution was extracted with ether and washed with saturated brine, and the resulting organic layer was dried on anhydrous sodium carbonate. Thereafter, the organic layer was filtered through silica gel (5 g), the solvent was removed by evaporation and then the resulting residue was purified by subjecting it to a silica gel column chromatography (ether) to obtain 650 mg (92.3%) of the title compound in the form of light yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728835uspto-grants-1998_03