反応 #459691

ord-63d8953766aa4f0cbfe1a08ea1c5c844

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A slight exothermic reaction
  2. 2
    その他to come to room temperature
  3. 3
    workup.DISTILLATIONthe reaction is distilled in vacuo
  4. 4
    その他boiling 96°-102°
  5. 5
    workup.DISTILLATIONUpon redistillation a boiling point of 90°-92°/0.1 mm
  6. 6
    その他is obtained

実験手順

To a stirred solution of 1-chloro-4-hydroxynonane (Example A, Step 2) (11.0 g., 0.062 mole) and dihydropyrane (5.2 g., 0.062 mole) cooled in an ice bath is added 5 drops of hydrochloric acid (conc.). A slight exothermic reaction is noted and when this is complete the reaction is allowed to come to room temperature, then stand for 2 hours. At the end of this period several pellets of sodium hydroxide are added and the reaction is distilled in vacuo. The yield of 1-chloro-4-(2-tetrahydropyranyloxy)nonane is 12.5 g. (77%), boiling 96°-102°/0.1 mm. Upon redistillation a boiling point of 90°-92°/0.1 mm. is obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04091107uspto-grants-1978_05