反応 #4524

反応方程式

1-chloroethylchloroformate

2,3-dihydro-2,2-dimethyl-7-benzofuranol

pyridine

→

1-chloroethyl 2,3-dihydro-2,2-dimethyl-7-benzofuranyl carbonate

収率 84.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度The mixture is cooled to between 0° and 5° C.
2. 2
   洗浄The organic phase is then washed with 2×50 ml of iced water
3. 3
   乾燥It is dried over magnesium sulphate
4. 4
   その他the solvent is evaporated
5. 5
   その他A yellow oil is obtained which
6. 6
   workup.DISTILLATIONis distilled
7. 7
   その他34.1 g of the expected carbonate is then recovered (84% yield)

実験手順

21.5 g (0.15 mole) of 1-chloroethylchloroformate are added in a single portion to a solution of 2,3-dihydro-2,2-dimethyl-7-benzofuranol (24.6 g; 0.15 mole) in dichloromethane (150 ml). The mixture is cooled to between 0° and 5° C., and 12 g (0.15 mole) of pyridine are added dropwise. The mixture is stirred for 3 hours at 20° C. The organic phase is then washed with 2×50 ml of iced water. It is dried over magnesium sulphate and the solvent is evaporated. A yellow oil is obtained which is distilled. 34.1 g of the expected carbonate is then recovered (84% yield).

出典