反応式
[CH2:1]([C:3]1([CH3:10])[NH:7][C:6](=[O:8])[NH:5][C:4]1=[O:9])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl:17][CH2:18][CH2:19]Cl>CN(C)C=O>[Cl:17][CH2:18][CH2:19][N:5]1[C:4](=[O:9])[C:3]([CH2:1][CH3:2])([CH3:10])[NH:7][C:6]1=[O:8]参加物
実験手順
284.3 g of 5-ethyl-5-methyl-hydantoin (2.0 mols), 138.2 g of anhydrous potassium carbonate (1.0 mol), 791.7 g of 1,2-dichloroethane (8.0 mols) and 230 ml of dimethylformamide are subjected to an azeotropic circulatory distillation for 25 hours at 90° C to 107° C internal temperature (external temperature: 160° C), in the manner described under Example 1 (a). After completion of the reaction, the mixture is filtered whilst still hot and the filtrate is concentrated on a rotary evaporator at 90° C under a waterpump vacuum. The reaction mixture is then dried to constant weight at 90° C and 10-1 mm Hg. 392.5 g of a brown, clear, product (95.9% of theory) are obtained, and are purified by vacuum distillation (boiling point0.2 : 147° C). Yield of pure product: 327.3 g (80% of theory). A sample recrystallised from diethyl ether melts at 58.0° C to 59.0° C.
後処理
- customAfter completion of the reaction
- filtrationthe mixture is filtered whilst still hot and the filtrate
- concentrationis concentrated on a rotary evaporator at 90° C under a waterpump vacuum
- customThe reaction mixture is then dried to constant weight at 90° C
- custom392.5 g of a brown, clear, product (95.9% of theory) are obtained
- distillationare purified by vacuum distillation (boiling point0.2 : 147° C)
- customA sample recrystallised from diethyl ether melts at 58.0° C to 59.0° C.
出典と根拠
- ORDレコード
- ord-7700069e5d894ef0a937aa950539c858
- 出典データセット
- uspto-grants-1976_11
- 特許番号
- US03994858
関連ノート
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