Trimethylsilyl cyanide → HCID 86741182, Verbindung

HRID 979800Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 979800
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH2:7][C:8]2=O.[Cl-].[Al+3].[Cl-].[Cl-].C[Si]([C:24]#[N:25])(C)C>C1C=CC=CC=1>[C:24]([CH2:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]=[CH:8]2)#[N:25]

Komponenten

5

Edukt 3

HCID 82115Trimethylsilyl cyanideHCID 6451240Aluminum(III) ChlorideHCID 82192465,6-dimethoxy-1-tetralone

Produkt 1

HCID 86741182HCID 86741182, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

5,6-dimethoxytetralone (20 g) was dissolved in benzene (20 ml) and trimethylsilyl cyanide (16 ml). A catalytic amount of aluminum chloride was added and the reaction heated at 70° C. under nitrogen for 30 minutes. The volatiles were removed in vacuo and methanol (20 ml) added. Gaseous hydrochloric acid was bubbled through the methanol solution for 30 minutes resulting in precipitation of a solid. Stirring was continued for 1 hour, then the mixture was filtered and dried affording 19.9 g. of product (96% yield); m.p. 138°-9° C.

Aufarbeitung

  1. customThe volatiles were removed in vacuo and methanol (20 ml)
  2. additionadded
  3. customGaseous hydrochloric acid was bubbled through the methanol solution for 30 minutes
  4. customresulting in precipitation of a solid
  5. filtrationthe mixture was filtered
  6. customdried
  7. customaffording 19.9 g

Quellen und Nachweise

ORD-Eintrag
ord-288484d9dbb34f1cbfe76439061ad0e6
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04634705

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