Reaction equation
CC(C)([O-])C.[K+].[C:7](I)([C:10]([C:13]([C:16]([C:19]([C:22]([F:25])([F:24])[F:23])([F:21])[F:20])([F:18])[F:17])([F:15])[F:14])([F:12])[F:11])([F:9])[F:8]>>[CH:7]([C:10]([C:13]([C:16]([C:19]([C:22]([F:23])([F:24])[F:25])([F:20])[F:21])([F:17])[F:18])([F:15])[F:14])([F:12])[F:11])([F:9])[F:8]Participants
Procedure
Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 400 cc of isopropyl alcohol (the water content in the isopropyl alcohol being not higher than 50 ppm, the same is true in the following Examples), and 84.2 g (0.75 mol) of potassium tert-butoxide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 223 g (0.5 mol) of C6F13I was dropwise added thereto over a period of two hours. After completion of the dropwise addition, heating and refluxing were continued for one hour. The conversion at that time was 100%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor and further washed five times with 200 g of water, to obtain 151 g of C6F13H having a purity of 99.8%. In the reactor, no formation of tar was observed.
Workup
- customInto a 1 l four-necked flask equipped with a stirrer
- distillationa distillation
- customapparatus-equipped
- temperaturereflux condenser, a dropping funnel
- additionwere charged
- temperatureThe reactor was heated
- customto 60° C
- additionAfter completion of the dropwise addition
- temperatureheating
- temperaturerefluxing
- waitwere continued for one hour
- distillationA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
- washfurther washed five times with 200 g of water
Sources & evidence
- ORD record
- ord-10f61eec01514446b12ab54de9e82bc4
- Source dataset
- uspto-grants-1997_04
- Patent number
- US05618986
Linked notes
Loading…