Réaction #10409

ord-80072c018d95452cb4a32b07e670454c

Conditions de réaction

Température
25°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe layers are separated
  2. 2
    Lavagethe aqueous layer is washed three times with ethyl acetate
  3. 3
    SéchageThe combined organic layers are dried over magnesium sulfate
  4. 4
    Concentrationconcentrated

Mode opératoire

2-Amino-4,5-difluorobenzoic acid, 2,2-dibenzylhydrazide (Example 15) (0.81 g, 2.2 mmol) and triphosgene (0.33 g, 1.1 mmol) are combined in 100 mL of methylene chloride and stirred at 25° C. for 20 hours. The solution is poured into 200 mL of saturated NaHCO3, the layers are separated, and the aqueous layer is washed three times with ethyl acetate. The combined organic layers are dried over magnesium sulfate and then concentrated to give 0.86 g of the title compound as a solid. MS CI: m/z 394 (MH+).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07094780B1uspto-grants-2006_08