反応式
C([O:3][CH:4](OCC)[CH2:5][CH2:6][N:7]1[C:13](=[O:14])[CH2:12][C:11]2[CH:15]=[C:16]([O:21][CH3:22])[C:17]([O:19][CH3:20])=[CH:18][C:10]=2[CH:9]=[CH:8]1)C.C(O)C>S(=O)(=O)(O)O>[CH3:20][O:19][C:17]1[C:16]([O:21][CH3:22])=[CH:15][C:11]2[CH2:12][C:13](=[O:14])[N:7]([CH2:6][CH2:5][CH:4]=[O:3])[CH:8]=[CH:9][C:10]=2[CH:18]=1参加物
実験手順
First, 3-(7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl)-propionaldehyde diethyl acetal (3.5 g, 0.01 mol) is heated in 2N sulphuric acid (50 ml) and ethanol (50 ml) to 40° C. for 2 hours. The alcohol is then distilled off in vacuo, the residue is made alkaline with saturated potassium carbonate solution with cooling and extracted several times with ethyl acetate. The ethyl acetate extract is extracted twice with sodium hydrogensulphite solution. The bisulphite extract is acidified with concentrated hydrochloric acid and heated for half an hour to 40° C. in vacuo in order to eliminate the sulphur dioxide. Then, saturated potassium carbonate solution is added and the mixture is extracted several times with methylene chloride, dried over magnesium sulphate and evaporated. Yield: 1.7 g. Mp: 95°-96° C.
後処理
- distillationThe alcohol is then distilled off in vacuo
- temperaturewith cooling
- extractionextracted several times with ethyl acetate
- extractionThe ethyl acetate extract
- extractionis extracted twice with sodium hydrogensulphite solution
- extractionThe bisulphite extract
- temperatureheated for half an hour to 40° C. in vacuo in order
- additionThen, saturated potassium carbonate solution is added
- extractionthe mixture is extracted several times with methylene chloride
- dry with materialdried over magnesium sulphate
- customevaporated
出典と根拠
- ORDレコード
- ord-7c522c6de0974f9ea436431392b948db
- 出典データセット
- uspto-grants-1986_04
- 特許番号
- US04584293
関連ノート
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