反応 #214850

ord-0d6962dd97ff4ef6a53330447d6bf967

反応方程式

CN1CC(=O)NC1=O
1-methylhydantoin
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C=COCCCl
2-chloroethyl vinyl ether
CN(C)C=O
dimethylformamide
C=COCCN1C(=O)CN(C)C1=O
1-Methyl-3-(2-vinyloxyethyl)-hydantoin

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他is reacted for 2 hours and 30 minutes at 130°-138° C.
  2. 2
    その他whilst removing
  3. 3
    その他the water of reaction
  4. 4
    その他are obtained
  5. 5
    workup.DISTILLATIONThe crude product is distilled (boiling point 133° C.-134° C./0.2 mm Hg) and 108.5 g (81.8% of theory) of a colourless, viscous distillate
  6. 6
    その他are obtained
  7. 7
    その他this crystallises

実験手順

A mixture of 82.6 g (0.72 mol) of 1-methylhydantoin, 50.7 g (0.37 mol) of anhydrous potassium carbonate, 89.6 g (0.84 mol) of 2-chloroethyl vinyl ether, 700 ml of dimethylformamide and 100 ml of toluene is reacted for 2 hours and 30 minutes at 130°-138° C., whilst removing the water of reaction. The mixture is then worked up as described in Example 1, and 128.5 g of a clear, reddish brown, viscous crude product (96.9% of theory) are obtained. The crude product is distilled (boiling point 133° C.-134° C./0.2 mm Hg) and 108.5 g (81.8% of theory) of a colourless, viscous distillate are obtained; this crystallises and melts at 54°-56° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04256867uspto-grants-1981_03