反応式
C[O-].[Na+].Cl.[CH3:5][NH:6][OH:7].[CH3:8][C:9](=[CH2:20])[CH2:10][N:11]([CH2:17][CH:18]=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13].O>CO.C1(C)C=CC=CC=1>[CH3:5][N:6]1[O:7][CH2:8][C:9]2([CH3:20])[CH:18]1[CH2:17][N:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:10]2参加物
実験手順
21.7 g of 30% strength sodium methylate solution are added dropwise to 10 g (0.12 mol) of N-Methylhydroxylamine hydrochloride in 26 ml of methanol. The sodium chloride is filtered off with suction and washed with 8 ml of methanol and 80 ml of toluene. This solution is added dropwise to 19.2 g (0.11 mol) of N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane, which is heated under reflux in 160 ml of toluene using a water separator. The mixture is heated under reflex overnight, the product is extracted with 160 ml of 10% strength hydrochloric acid and the hydrochloric acid solution is rendered alkaline with potassium carbonate and extracted with six portions, of 200 ml of CHCl3. The extracts are dried over K2CO3 and concentrated and the residue is distilled.
後処理
- filtrationThe sodium chloride is filtered off with suction
- washwashed with 8 ml of methanol and 80 ml of toluene
- temperatureis heated
- temperatureThe mixture is heated under reflex overnight
- extractionthe product is extracted with 160 ml of 10% strength hydrochloric acid
- extractionextracted with six portions, of 200 ml of CHCl3
- dry with materialThe extracts are dried over K2CO3
- concentrationconcentrated
- distillationthe residue is distilled
出典と根拠
- ORDレコード
- ord-5c9a80430a6a40dd9c22f32291c40544
- 出典データセット
- uspto-grants-1997_03
- 特許番号
- US05607942
関連ノート
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