반응 #214849

반응 방정식

5-methyl-5-ethylhydantoin

2-chloroethyl vinyl ether

potassium carbonate

→

3-[2-(Vinyloxy)-ethyl]-5-methyl-5-ethyl-hydantoin

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   여과the reaction mixture is filtered
3. 3
   농축the clear filtrate is concentrated on a rotary evaporator at 80° C. under vacuum from a waterpump
4. 4
   workup.ADDITION2 g of active charcoal are added
5. 5
   workup.WAITthe mixture is kept at the boil for 15 minutes
6. 6
   여과It is then filtered
7. 7
   농축the filtrate is concentrated on a rotary evaporator at 60° C. under vacuum from a waterpump
8. 8
   기타is freed from non-volatile constituents at 60° C.
9. 9
   기타0.5 mm Hg and 86.9 g (81.9% of theory) of a yellowish, viscous crude product are obtained
10. 10
    workup.DISTILLATIONThis is purified by distillation in a high vacuum and 80.34 g (75.7% of theory) of the desired product, of boiling point 132° C./0.2 mm Hg
11. 11
    기타are obtained

실험 절차

A mixture of 71.04 g (0.5 mol) of 5-methyl-5-ethylhydantoin, 55.94 g (0.5 mol+5% excess) of 2-chloroethyl vinyl ether, 36.28 g (0.25 mol+5% excess) of anhydrous potassium carbonate and 150 ml of dimethylformamide is stirred, analogously to Example 1, for 4 hours and 35 minutes at 122°-129° C. After completion of the reaction, the reaction mixture is filtered and the clear filtrate is concentrated on a rotary evaporator at 80° C. under vacuum from a waterpump. The residue is taken up in 200 ml of acetone, 2 g of active charcoal are added and the mixture is kept at the boil for 15 minutes. It is then filtered and the filtrate is concentrated on a rotary evaporator at 60° C. under vacuum from a waterpump. The residue is freed from non-volatile constituents at 60° C. and 0.5 mm Hg and 86.9 g (81.9% of theory) of a yellowish, viscous crude product are obtained. This is purified by distillation in a high vacuum and 80.34 g (75.7% of theory) of the desired product, of boiling point 132° C./0.2 mm Hg, are obtained.

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