Water → HCID 18401890, Verbindung

HRID 1018660Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1018660
[CH:1]1[C:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:5]=2[CH:4]=[CH:3][C:2]=1[OH:12].C([O-])([O-])=O.[Cs+].[Cs+].Br[CH2:20][CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.O>CN(C=O)C>[CH:21]1([CH2:20][O:12][C:2]2[CH:3]=[CH:4][C:5]3[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[CH:1]=2)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 10796Cesium carbonateHCID 137636Cyclohexane, (bromomethyl)-HCID 108882365H-Benzocyclohepten-2-ol, 6,7,8,9-tetrahydro-

Produkt 1

HCID 18401890HCID 18401890, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a mixture of 6,7,8,9-tetrahydro-5H-benzocyclohepten-2-ol (Helvetica Chimica Acta 1947, 1883.) (9.9 g, 61.0 mmol) and Cs2CO3 (26.3 g, 73.2 mmol) in DMF (100 ML) was added (bromomethyl)cyclohexane (10.2 mL, 73.2 mmol). The mixture was heated to 60° C. for 18 h, dumped into water and extracted with ethyl acetate. The combined extracts were washed with water, dried over magnesium sulfate and concentrated to a solid. The solid was recrystallized from ethanol (13.0 g, 83%). m.p. 62-63° C.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe combined extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated to a solid
  5. customThe solid was recrystallized from ethanol (13.0 g, 83%)

Quellen und Nachweise

ORD-Eintrag
ord-75597b37e63141ccac0cacb19b604733
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06482852B2

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