反応式
Cl.[CH:2](=[NH:6])[O:3][CH2:4][CH3:5].Cl.[F:8][C:9]([F:13])([F:12])[CH2:10]N.C(=O)([O-])[O-].[K+].[K+].O>C(Cl)Cl>[F:8][C:9]([F:13])([F:12])[CH2:10][N:6]=[CH:2][O:3][CH2:4][CH3:5]参加物
6
実験手順
Ethyl formimidate hydrochloride (0.555 g, 5 mmole), 2,2,2-trifluoroethylamine hydrochloride (0.677 g, 5 mmole) and potassium carbonate (0.345 g, 2.5 mmole) are suspended in 20 ml CH2Cl2 and treated with 1 ml H2O. The mixture is shaken vigorously for 3 minutes. The organic phase is separated and the aqueous extracted twice with 10 ml portions of CH2Cl2. The combined organic phase is dried and the CH2Cl2 distilled through a Vigreauxe column to give the Ethyl N-(2,2,2-trifluoroethyl)formimidate. n.m.r. δ1.333 t (CH3CH2); 3.8 q (j=10 c.p.s., CF3CH2) 4.23 q (j=7.5, CH3CH2O); 7.6 S (H--C=N).
後処理
- customThe organic phase is separated
- extractionthe aqueous extracted twice with 10 ml portions of CH2Cl2
- customThe combined organic phase is dried
- distillationthe CH2Cl2 distilled through a Vigreauxe column
出典と根拠
- ORDレコード
- ord-10ed42efae734893945049ee38c86671
- 出典データセット
- uspto-grants-1980_11
- 特許番号
- US04232030
関連ノート
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