تفاعل #10035

ord-3d53efdb7a5449338c2b2634ab6dd476

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction mixture is stirred at 5° C. for 15 minutes
  2. 2
    درجة الحرارةThe mixture is warmed to 80° C.
  3. 3
    workup.STIRRINGunder stirring for about 24 hours

الإجراء التجريبي

To a solution of N-methylformanilide (30 g), butyl vinyl ether (22.2 g) in 15 ml of acetonitrile under stirring at 5° C., a solution of bis-trichloromethylcarbonate (26.1 g) in 70 ml of acetonitrile is added dropwise in 80 min. The reaction mixture is kept under stirring at 5° C. overnight, then phosphorus oxychloride (31.4 g) is added dropwise in 30 minutes, then the reaction mixture is stirred at 5° C. for 15 minutes. 3-[3-(4-Fluorophenyl)-1-(1-Methylethyl)-1H-Indole (35.8 g) and acetonitrile (25 ml) are added. The mixture is warmed to 80° C. and kept under stirring for about 24 hours. The reaction mixture is worked up as described in Example 3b to give the product (69% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091382B2uspto-grants-2006_08