Реакция #10409

ord-80072c018d95452cb4a32b07e670454c

Растворители

Условия реакции

Температура
25°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe layers are separated
  2. 2
    Промывкаthe aqueous layer is washed three times with ethyl acetate
  3. 3
    СушкаThe combined organic layers are dried over magnesium sulfate
  4. 4
    Концентрированиеconcentrated

Методика

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+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07094780B1uspto-grants-2006_08