反応 #315322

ord-64bb2ba12ad44990b796d89a7af372cf

反応方程式

OCCCCCCBr
6-bromo-1-hexanol
C1=COCCC1
dihydropyran
BrCCCCCCOC1CCCCO1
6-bromo-1-(tetrahydropyranyloxy)hexane
収率 91.1%

試薬

なし

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled to 5° C. or less
  2. 2
    その他were dripped at a temperature of 10° C. or less
  3. 3
    その他a reaction
  4. 4
    その他Residues obtained by this reaction
  5. 5
    その他were purified by silica gel column with hexane/IPE (diisopropylether)=5/1

実験手順

First, 197.8 g (1.09 mol) of 6-bromo-1-hexanol were fed into a 500 mL reactor vessel and cooled to 5° C. or less, and further 102.1 g (1.21 mol) of dihydropyran were dripped at a temperature of 10° C. or less. After completion of dripping, the mixture was warmed to room temperature to carry out a reaction under stirring for one hour. Residues obtained by this reaction were purified by silica gel column with hexane/IPE (diisopropylether)=5/1, and thus 263.4 g of 6-bromo-1-(tetrahydropyranyloxy)hexane were obtained. The yield was 90.9%. Formula (26) below shows the reaction formula of the step 1.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07560731B2uspto-grants-2009_07