تفاعل #79075

ord-723a1fd0b17e41cbb04c9b79421faa5d

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
195°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe resulting product is then chromatographed over silica gel (5-100. EtOH/EtOAc)

الإجراء التجريبي

A mixture of 7-amino-4-methylthiopyrido[4,3-d]pyrimidine (234 mg, 1.22 mmol) (described in a previous experimental) and 3-aminobenzotrifluoride (2.00 mL, 16.0 mmol) is stirred under N2 at 190-200° C. for 2 h, and the resulting product is then chromatographed over silica gel (5-100. EtOH/EtOAc), and then over alumina (5-7%. EtOH/CHCl3) to give 7-amino-4-(3-trifluoromethylanilino)pyrido[4,3-d]pyrimidine (157 mg, 42%) as a cream solid. 1H NMR (DMSO) δ 10.04 (1H, s), 9.37 (1H, s), 8.46 (1H, s), 8.31 (1H, s), 8.19 (1H, d, J=8.2 Hz), 7.62 (1H, t, J=8.0 Hz), 7.45 (1H, d, J=7.7 Hz), 6.69 (2H, brs), 6.47 (1H, s).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06713484B2uspto-grants-2004_03