反応 #315324

反応方程式

6-bromo-1-hexanol

dihydropyran

→

6-bromo-1-(tetrahydropyranyloxy)hexane

収率 91.1%

反応条件

後処理

1. 1
   温度cooled to 5° C. or less
2. 2
   その他were dripped at 10° C. or less
3. 3
   その他purified

実験手順

6-bromo-1-(tetrahydropyranyloxy)hexane was synthesized in the same manner as in Example 1 (the formula (26): step 1). 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 then 102.1 g (1.21 mol) of dihydropyran were dripped at 10° C. or less. After completion of dripping, the mixture was warmed to room temperature and stirred for one hour. The obtained residues were subjected to silica gel column and purified using a mixed solvent of hexane/diisopropylether (IPE) (volume ratio 5:1) as an eluting solvent, and thus 263.4 g of 6-bromo-1-(tetrahydropyranyloxy)hexane were obtained. The yield in this case was 90.9%.

出典