Reacción #3754

ord-08dfdae2443b4d4698992a68f3846a73

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling to 0° C.
  2. 2
    OtroAdd water (100 ml) and collect the resulting precipitate
  3. 3
    Filtraciónby suction filtration
  4. 4
    OtroPurify the white solid by flash chromatography (50% ethyl acetate/hexane)
  5. 5
    Otrotriturate with 5% diethyl ether/hexane
  6. 6
    Otroto provide
  7. 7
    Secadoafter drying under vacuum at 120° C. for 30 minutes the title compound (1.04 g), m.p. 202°-204° C.

Procedimiento

Dissolve 1,2,3,4-tetrahydronaphthalene-2-carboxylic acid (2-amino-4,6-dioxo-3,5-dipropylcyclohex-1-enyl)amide (2.0 g, 5.2 mmol) in ethanol (50 ml), add 15% potassium hydroxide (50 ml) and heat to 70° C. for 4 hours. After cooling to 0° C., acidify the reaction with concentrated hydrochloric acid (13 ml). Add water (100 ml) and collect the resulting precipitate by suction filtration. Purify the white solid by flash chromatography (50% ethyl acetate/hexane) and triturate with 5% diethyl ether/hexane to provide, after drying under vacuum at 120° C. for 30 minutes the title compound (1.04 g), m.p. 202°-204° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05734052uspto-grants-1998_03