反応 #81902

ord-26a020e1e80a4d4c857431a3c9c2b02f

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated to reflux
  2. 2
    温度The resulting solution was maintained
  3. 3
    温度at reflux for 20 minutes
  4. 4
    濃縮concentrated at atmospheric pressure to about 0.25 mL volume
  5. 5
    workup.ADDITIONdiluted with diethyl ether (1 mL)
  6. 6
    ろ過The separated crystals were filtered
  7. 7
    洗浄washed with diethyl ether

実験手順

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.; MS (CI) 363 (M+ +1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05620981uspto-grants-1997_04