반응 #2372072

반응 방정식

2-chloroethyl vinylether

Sodium hydroxide

bis(4-hydroxyphenyl)phenylsulfonium triflate

DMSO

diethyl ether

ether

→

bis(4-vinyloxyethyloxyphenyl)phenylsulfonium triflate

수율 61.5%

용매

DI water

반응 조건

후처리

1. 1
   기타A 3-neck-round bottom flask was fitted with a condenser, an addition funnel
2. 2
   온도The temperature was then increased to 80° C.
3. 3
   온도to cool down to room temperature
4. 4
   기타to form three layers
5. 5
   세척to wash the ether solution 3 times
6. 6
   기타An oily layer was collected
7. 7
   농축concentrated to dryness

실험 절차

A 3-neck-round bottom flask was fitted with a condenser, an addition funnel, nitrogen source, and a magnetic bar. Sodium hydroxide (8.64 g, 0.216 mol), bis(4-hydroxyphenyl)phenylsulfonium triflate (16 g, 0.036 mol) and DMSO (90 ml) were added to a round bottom flask under N2. The mixture was heated to 60° C. for 1 hour. 2-chloroethyl vinylether (23 g, 0.216 mol) was added dropwise to the mixture via the addition funnel. The temperature was then increased to 80° C. and the reaction was held at that temperature for 5 hours. The reaction mixture was then allowed to cool down to room temperature. Thereafter, the reaction mixture was poured into diethyl ether to form three layers: aqueous, ether, and an oil. DI water was used to wash the ether solution 3 times. An oily layer was collected and concentrated to dryness. 12.9 g (61.5%) of bis(4-vinyloxyethyloxyphenyl)phenylsulfonium triflate was obtained. The structure was confirmed using 1H and 19F NMR.

출처