تفاعل #45670

ord-b781b3d8c25744e5908d183c004c4eaf

المذيبات

ظروف التفاعل

درجة الحرارة
130°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    ترشيحthe precipitated solid was collected by filtration
  3. 3
    غسيلwashed in diethyl ether

الإجراء التجريبي

Under nitrogen atmosphere, a mixture of 2-amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (6.67 g, 27.2 mmol) and ethyl triethoxyacetate (24.0 g, 54.4 mmol) was stirred at 130° C. for 15 hours. After cooling, n-hexane was added to the reaction liquid, and the precipitated solid was collected by filtration. The obtained solid was suspended and washed in diethyl ether to obtain the entitled compound (7.10 g, 80%) as a pale dark brown solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737166B2uspto-grants-2010_06