1,4-Dichlorobutane → HCID 11665882, Verbindung

HRID 253687

Reaktionsgleichung

Reaktionsgleichung von HRID 253687
[OH:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:18][CH2:19][CH2:20][CH2:21][CH2:22]Cl>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:18][CH2:19][CH2:20][CH2:21][CH2:22][O:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 80591,4-DichlorobutaneHCID 11430Potassium CarbonateHCID 70206596-Hydroxy-1-indanone

Produkt 1

HCID 11665882HCID 11665882, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 74236Tetrabutylammonium BromideKatalysator

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

Mixture of 6-hydroxyindan-1-one of the formula (11) (20 gm, 0.135 mol), potassium carbonate (40 gm, 0.289 mol), 1,4-dichlorobutane (80 ml, 0.73 mol) and tetrabutyl ammonium bromide (2 g) was stirred for 1-3 hrs at 95° C. then distilled off excess 1,4-dichloro butane, diluted with water (80 ml). The aqueous layer was extracted with ethyl acetate, and the extract was washed with water, dried and evaporated off under reduced pressure to dryness. The evaporation residue is purified by crystallization using isopropyl ether as a solvent gave 29.5 gm of novel 6-(4-CHLORO BUTOXY)-INDAN-1-ONE of the formula (3).

Aufarbeitung

  1. distillationthen distilled off excess 1,4-dichloro butane
  2. additiondiluted with water (80 ml)
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe extract was washed with water
  5. customdried
  6. customevaporated off under reduced pressure to dryness
  7. customThe evaporation residue is purified by crystallization

Quellen und Nachweise

ORD-Eintrag
ord-1fb0f1f6a264471896e071da46f411ec
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07872132B2

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