反応 #511485

ord-c7763484ead34970ac2552da47af3675

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwise added
  2. 2
    workup.ADDITIONAfter complete addition
  3. 3
    ろ過the white precipitate was filtered off
  4. 4
    洗浄washed twice with 100 ml of +4° C.
  5. 5
    温度pre-cooled diethylether
  6. 6
    その他dried

実験手順

To an ice-cooled mixture of 4-hydroxybenzoic acid (13.81 g) in 250 ml of diethylether containing 1.98 g of pyridinium p-toluenesulphonic acid, 3,4-dihydro-2H-pyran (16 g) was drop wise added. After complete addition stirring was continued at temperature below +8° C. for 4 h and the white precipitate was filtered off, washed twice with 100 ml of +4° C. pre-cooled diethylether and dried to give nearly pure 4-(tetrahydro-2H-pyran-2-yloxy)benzoic acid as white powder.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08105662B2uspto-grants-2012_01