반응 #81699

반응 방정식

methanol

sodium methoxide

C8F17I

→

C8F17H

수율 95.7%

용매

water

반응 조건

후처리

1. 1
   기타Into a 500 cc four-necked equipped with a stirrer, a reflux condenser, a dropping funnel
2. 2
   온도The reactor was heated
3. 3
   기타to 60° C
4. 4
   workup.ADDITIONAfter completion of the dropwise addition
5. 5
   온도heating
6. 6
   온도refluxing
7. 7
   workup.WAITwere continued for 10 hours
8. 8
   workup.DISSOLUTIONto dissolve
9. 9
   기타precipitated potassium iodide
10. 10
    기타The crude reaction solution
11. 11
    기타was separated into two layers
12. 12
    세척the fluorocarbon layer (lower layer) was further washed with 300 g of water

실험 절차

Into a 500 cc four-necked equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol and 32.4 g (0.6 mol) of sodium methoxide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 273 g of (0.5 mol) of C8F17I was dropwise added thereto over a period of one hour. After completion of the dropwise addition, heating and refluxing were continued for 10 hours. The conversion at that time was 99.8%. The reactor was cooled to room temperature. Then, 300 g of water was added to dissolve precipitated potassium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed with 300 g of water to obtain 201 g of C8F17H having a purity of 99.4%. In the reactor, no formation of tar was observed.

출처