تفاعل #10409

ord-80072c018d95452cb4a32b07e670454c

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe layers are separated
  2. 2
    غسيلthe aqueous layer is washed three times with ethyl acetate
  3. 3
    تجفيفThe combined organic layers are dried over magnesium sulfate
  4. 4
    تركيزconcentrated

الإجراء التجريبي

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+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07094780B1uspto-grants-2006_08