Reacción #417901

ord-523b9c4e97b643f8ad5dbfb9b5aeeea5

Ecuación de reacción

O=P(Cl)(Cl)Cl
phosphoryl chloride
[O-][n+]1ccnc2c3ccccc3c3ccccc3c21
dibenzo[f,h]quinoxaline-1-oxide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Clc1cnc2c3ccccc3c3ccccc3c2n1
2-Chloro-Dibenzo[f,h]Quinoxaline
Rendimiento 93.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroobtained in the above Step 1
  2. 2
    Temperaturawhile being heated
  3. 3
    Temperaturaunder reflux for 1 hour
  4. 4
    FiltraciónThis solution was filtered
  5. 5
    Lavadothe obtained residue was washed with water
  6. 6
    Otromethanol to give
  7. 7
    Otrothe object of the synthesis (as a pale yellow powder in a yield of 93%)
  8. 8
    OtroThe synthesis scheme of Step 2

Procedimiento

Next, 18 mL of phosphoryl chloride was dripped into 2.91 g of dibenzo[f,h]quinoxaline-1-oxide obtained in the above Step 1. This mixed solution was stirred while being heated under reflux for 1 hour. This mixed solution was poured into iced water, followed by addition of potassium carbonate so that the mixture was alkaline. This solution was filtered, and the obtained residue was washed with water and then methanol to give the object of the synthesis (as a pale yellow powder in a yield of 93%). The synthesis scheme of Step 2 is illustrated in the following (a″′-2-2).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08877351B2uspto-grants-2014_11