Water → Thioxanthene

HRID 581647

Reaktionsgleichung

Reaktionsgleichung von HRID 581647
[CH:1]1[C:14]2[C:13](=O)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].CCOCC.O>C1C=CC=CC=1>[CH:1]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 3283Diethyl EtherHCID 10295ThioxanthoneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 67495ThioxantheneAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A solution of thioxanthone (10 g) in 60 mL of benzene was treated with 5.0 g of LAH by stirring for 15 min. The mixture was heated and 100 mL of ether was added carefully. Reflux was continued for 90 min. The cooled mixture was neutralized with water. The solids were filtered off and the filtrate evaporated to dryness. Pure thioxanthene (9.1 g, 98%) was isolated by chromatography using 20% ethyl acetate/hexane; 1H NMR (CDCl3) δ 3.82 (s, 3H), 7.21 (m, 4H), 7.33 (m, 2H), 7.46 (m, 2H).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureReflux
  3. waitwas continued for 90 min
  4. filtrationThe solids were filtered off
  5. customthe filtrate evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-4a728b20ca324bcdb9d8d56c9eb6c534
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05922558

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