Ethyl [(phenoxycarbonyl)oxy]acetate → 2-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylate

HRID 2242933Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2242933
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.C1([O:21][C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=O)C=CC=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][N:12]([C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:21])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 12094709Ethyl [(phenoxycarbonyl)oxy]acetateHCID 126455664-(4-Bromophenoxy)piperidine

Produkt 1

HCID 674168332-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylateAusbeute 99,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

2.7 g (7.58 mmol) of 4-[(4-bromophenyl)-oxy]piperidine, prepared in Step 4.2, and 1.70 g (7.6 mmol) of ethyl {[(phenyloxy)carbonyl]oxy}acetate, prepared in accordance with Example 1.1, are mixed in 40 ml of toluene and the solution is heated at 50° C. for 20 hours. After cooling, it is evaporated to dryness and the product is purified by chromatography on silica gel, eluting with a 40/60 mixture of ethyl acetate and cyclohexane. The eluate is subsequently triturated in diisopropyl ether, to give 2.9 g of product in powder form.

Aufarbeitung

  1. customprepared in accordance with Example 1.1
  2. temperatureAfter cooling
  3. customit is evaporated to dryness
  4. customthe product is purified by chromatography on silica gel
  5. washeluting with a 40/60 mixture of ethyl acetate and cyclohexane
  6. customThe eluate is subsequently triturated in diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-81afad4f08c84058abee8c63369f8144
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07674805B2

Notizen zur Reaktion

Wird geladen…