18-Crown-6 → N-chloroacetyl-N-methylcarbamoyl fluoride
反応式
[Cl:1][CH2:2][C:3]([N:5]([CH3:9])[C:6](Cl)=[O:7])=[O:4].[F-:10].[K+].C1OCCOCCOCCOCCOCCOC1>ClCCl>[Cl:1][CH2:2][C:3]([N:5]([CH3:9])[C:6]([F:10])=[O:7])=[O:4]参加物
5
実験手順
A mixture of 10.0 g of N-Chloroacetyl-N-methylcarbamoyl chloride, 3.8 g of anhydrous potassium fluoride and 0.5 g of 18-crown-6 in 50 cc of dichloromethane was stirred at room temperature under nitrogen for about 16 hours. The liquid was decanted and the residue was extracted with 50 cc dichlormethane. The dichloromethane layers were combined and the solvent stripped off to afford 9.0 g. (Yield 100%) of N-chloroacetyl-N-methylcarbamoyl fluoride. The product was further purified by distillation under reduced pressure. B.p. 59° C./0.2 mm.
後処理
- customThe liquid was decanted
- extractionthe residue was extracted with 50 cc dichlormethane
- customto afford 9.0 g
出典と根拠
- ORDレコード
- ord-004ef200fc5841ada6f0de7397b9b257
- 出典データセット
- uspto-grants-1987_01
- 特許番号
- US04637901
反応ノート
読み込み中…