Ethanol → Ethyl (2-chlorobenzoyl)acetate

HRID 986231

Reaktionsgleichung

Reaktionsgleichung von HRID 986231
[H-].[Na+].[C:3](=[O:10])([O:7][CH2:8][CH3:9])OCC.[Cl:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=[O:20])[CH3:19].C(O)C>O1CCCC1>[Cl:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18]([CH2:19][C:3]([O:7][CH2:8][CH3:9])=[O:10])=[O:20]

Komponenten

6

Edukt 4

HCID 702Ethanol2×HCID 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 72864Ethanone, 1-(2-chlorophenyl)-

Produkt 1

HCID 292405Ethyl (2-chlorobenzoyl)acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Sodium hydride (8.7 grams) and 21.4 grams of diethyl carbonate are suspended in 100 ml of tetrahydrofuran, 14 grams of o-chloroacetophenone is gradually dropped thereinto by keeping the inner temperature at 40° to 50° C., then a small amount of ethanol is added thereto and heated to reflux for four hours. After cooling, 20 ml of ethanol is added thereto, the mixture is poured into ice water, and extracted with ether. Ether extracts are combined, washed with water, dried with anhydrous magnesium sulfate, and ether is evaporated therefrom. The resulting oil is purified by distillation in vacuo to give 8.8 grams of colorless, oily product, b.p. 120° to 125° C./1 mmg Hg.

Aufarbeitung

  1. customat 40° to 50° C.
  2. temperatureheated
  3. temperatureto reflux for four hours
  4. temperatureAfter cooling
  5. extractionextracted with ether
  6. washwashed with water
  7. dry with materialdried with anhydrous magnesium sulfate, and ether
  8. customis evaporated
  9. distillationThe resulting oil is purified by distillation in vacuo
  10. customto give 8.8 grams of colorless, oily product, b.p. 120° to 125° C./1 mmg Hg

Quellen und Nachweise

ORD-Eintrag
ord-3823c647e0a742aa85112ba7366a48a0
Quelldatensatz
uspto-grants-1987_12
Patentnummer
US04711898

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