反応 #214849

反応方程式

5-methyl-5-ethylhydantoin

2-chloroethyl vinyl ether

potassium carbonate

→

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

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   ろ過the reaction mixture is filtered
3. 3
   濃縮the 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
   ろ過It is then filtered
7. 7
   濃縮the filtrate is concentrated on a rotary evaporator at 60° C. under vacuum from a waterpump
8. 8
   その他is freed from non-volatile constituents at 60° C.
9. 9
   その他0.5 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
    その他are obtained

実験手順

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.

出典