反应 #10409

ord-80072c018d95452cb4a32b07e670454c

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the layers are separated
  2. 2
    洗涤the aqueous layer is washed three times with ethyl acetate
  3. 3
    干燥The combined organic layers are dried over magnesium sulfate
  4. 4
    浓缩concentrated

实验过程

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+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07094780B1uspto-grants-2006_08