反応 #344429

反応方程式

1,2-dichloro-1,1,2,3,3,4,4,-heptafluoro-6-iodohexane

ethanol

potassium hydroxide

ethanol

→

desired product

収率 92.0%

5,6-DICHLORO-3,3,4,4,5,6,6-HEPTAFLUORO-1-HEXENE

収率 92.0%

溶媒

water

water

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   温度the reaction mixture was refluxed for 1 hour
3. 3
   その他Lower layer was separated
4. 4
   洗浄washed with water

実験手順

To a stirred solution of 1,2-dichloro-1,1,2,3,3,4,4,-heptafluoro-6-iodohexane (370.0 g) and ethanol (400 mL) was added dropwise a solution of potassium hydroxide (56.0 g), ethanol (300 mL) and water (20 mL) at 80°-90° C. over 40 minutes. After the addition was complete, the reaction mixture was refluxed for 1 hour and then poured into water. Lower layer was separated and washed with water to give desired product (233.5 g). 19F NMR: -63.9 (m, 2F), -111.9 (m, 2F), -116.2 (m, 2F), -130.5 (m, 1F); 1H NMR: 5.72 to 6.10 (m). IR: 1651 (m), 1422 (s), 1180 (s), 1055 (s), 1019 (s), 1002 (s), 980 (s).

出典