HCID 20161193, Verbindung → HCID 20161200, Verbindung

HRID 247017Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 247017
O[C:2]1([C:15]#[N:16])[CH2:10][C:9]2[C:4](=[CH:5][C:6]([O:13][CH3:14])=[C:7]([O:11][CH3:12])[CH:8]=2)[CH2:3]1>Cl>[CH3:14][O:13][C:6]1[CH:5]=[C:4]2[C:9](=[CH:8][C:7]=1[O:11][CH3:12])[CH2:10][C:2]([C:15]#[N:16])=[CH:3]2

Komponenten

3

Edukt 1

HCID 20161193HCID 20161193, Verbindung

Produkt 1

HCID 20161200HCID 20161200, VerbindungAusbeute 80,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

The crude alcohol (17.1 g) was suspended in hydrochloric acid (5M, 170 ml) and the mixture was stirred and heated to 75° C. After 30 min. the dark solution was cooled in an ice-bath and the resultant green solid was filtered off and dried at 60° C. The product was dissolved in dichloromethane and the solution was passed through a column of coarse silica (0.2-0.5 mm, Merck, 80 g). The appropriate fractions were combined and evaporated to dryness to give 5,6-dimethoxy-1H-indene-2-carbonitrile (12.6 g), m.p. 140°-141° C.

Aufarbeitung

  1. temperatureAfter 30 min. the dark solution was cooled in an ice-bath
  2. filtrationthe resultant green solid was filtered off
  3. customdried at 60° C
  4. dissolutionThe product was dissolved in dichloromethane
  5. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-b2e11faffd634216adb7d3266e55c54e
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04705782

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