反応 #459852

ord-36e9b06b696d4de498ca740a514f1285

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONhas been completely dissolved
  2. 2
    温度the mixture is refluxed for 3 hours
  3. 3
    その他The resulting reaction mixture
  4. 4
    洗浄is washed with a small amount of water
  5. 5
    濃縮the ethereal layer is concentrated
  6. 6
    その他to separate out crystals, which
  7. 7
    その他are recrystallized from ethanol

実験手順

A 36.3 g quantity of n-hexadecanol is dissolved in 200 ml of absolute ether, 3.3 g of metal sodium is added to the solution and the mixture is refluxed until the sodium has been completely dissolved. Subsequently 8.5 g of 2,4-dichloro-5-fluoropyrimidine is added to the solution, and the mixture is refluxed for 3 hours. The resulting reaction mixture is washed with a small amount of water, and the ethereal layer is concentrated to separate out crystals, which are recrystallized from ethanol to give 18.6 g of white crystalline 2,4-di(n-hexadecyloxy)-5-fluoropyrimidine in a yield of 63.1%, m.p. 62°-63° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04092313uspto-grants-1978_05