تفاعل #3262

ord-040121136d37435a8bcc1f1ef88ef22c

ظروف التفاعل

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

المعالجة

  1. 1
    درجة الحرارةwas heated to reflux
  2. 2
    درجة الحرارةThe resulting solution was maintained
  3. 3
    درجة الحرارةat reflux for 20 minutes
  4. 4
    تركيزconcentrated at atmospheric pressure to about 0.25 mL volume
  5. 5
    workup.ADDITIONdiluted with diethyl ether (1 mL)
  6. 6
    ترشيحThe separated crystals were filtered
  7. 7
    غسيلwashed with diethyl ether

الإجراء التجريبي

A mixture of 64.2 mg (0.20 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one (from Example 12) and 1 mL of acetic anhydride was heated to reflux. The resulting solution was maintained at reflux for 20 minutes and concentrated at atmospheric pressure to about 0.25 mL volume. The solution was cooled to 25° C. and diluted with diethyl ether (1 mL). The separated crystals were filtered and washed with diethyl ether to provide N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl]acetamide, wt 44.0 mg; mp 258°-260° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733914uspto-grants-1998_03