Magnesium orthosilicate → 2-Cyano-3dimethylamino-1-thien-3-ylpropen-1-one

HRID 345968

Reaktionsgleichung

Reaktionsgleichung von HRID 345968
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[O:10][N:9]=[CH:8][CH:7]=2)=[CH:2]1.CO[CH:13](OC)[N:14]([CH3:16])[CH3:15].[Si]([O-])([O-])([O-])[O-].[Mg+2].[Mg+2]>C(Cl)Cl>[CH3:16][N:14]([CH:13]=[C:7]([C:6](=[O:10])[C:3]1[CH:4]=[CH:5][S:1][CH:2]=1)[C:8]#[N:9])[CH3:15]

Komponenten

5

Edukt 3

HCID 66225Magnesium orthosilicateHCID 78373Dimethylformamide dimethyl acetalHCID 185168865-(Thiophen-3-yl)isoxazole

Produkt 1

HCID 299434852-Cyano-3dimethylamino-1-thien-3-ylpropen-1-oneAusbeute 56,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 41.2 g of 5-(3-thienyl)isoxazole and 36.0 g of dimethylformamide dimethylacetal, under nitrogen, is heated on a stream bath for 4 hours. The reaction is concentrated in vacuo to give a viscous oil which solidified. The residue is dissolved in methylene chloride and passed thru a short column of hydrous magnesium silicate. On cooling, 31.76 g of the desired product is obtained, mp 118°-119°, CI-MS:m/z 206(M30). Concentrating in vacuo the methylene chloride gives an additional 20.2 g of product. (Total recovered 51.96 g, 92%).

Aufarbeitung

  1. temperatureunder nitrogen, is heated on a stream bath for 4 hours
  2. concentrationThe reaction is concentrated in vacuo
  3. customto give a viscous oil which
  4. temperatureOn cooling

Quellen und Nachweise

ORD-Eintrag
ord-c173186a7e67482f8013b66cca805112
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05059709

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