反応 #61841

ord-4a542a07cdbf48b783167e4decab0fd8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度To a cooled
  2. 2
    workup.WAITthe mixture left for a further hour
  3. 3
    洗浄The mixture was washed twice with brine
  4. 4
    乾燥dried with sodium sulphate
  5. 5
    ろ過filtered
  6. 6
    その他evaporated in vacuo

実験手順

To a cooled (ice/salt bath) mixture of 2-amino-4-(naphth-1-yl)oxazole (1)(0.5 g) and triethylamine (0.8 ml) in anhydrous dichloromethane (5 ml) was added dropwise acetyl chloride (0.2 ml) over a minute. The resulting mixture was warmed to room temperature and left overnight. Further acetyl chloride (0.1 ml) was added and the mixture left for a further hour. Dichloromethane (40 ml) and few drops of methanol were added. The mixture was washed twice with brine, dried with sodium sulphate, filtered and evaporated in vacuo. The title compound (9) (0.35 g; m.p. 188-190° C.) was obtained following silica gel column chromatography of the residue in 2% methanol in chloroform.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07429607B2uspto-grants-2008_09