反応式
[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][N:6]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[CH2:14][CH2:13][C:12]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]1=2.Cl.C(=O)([O-])[O-].[K+].[K+].[CH2:28]([O:30][P:31](Cl)([O:33][CH2:34][CH3:35])=[O:32])[CH3:29]>CN(C=O)C>[CH2:28]([O:30][P:31]([N:2]([CH2:3][CH2:4][CH2:5][N:6]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=2[CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]1=2)[CH3:1])(=[O:32])[O:33][CH2:34][CH3:35])[CH3:29]参加物
実験手順
Desipramine hydrochloride (1 equivalent, 0.5 gram) was added drop wise to a stirred solution of potassium carbonate (2 equivalents, 0.456 gram) in dry DMF at 0° C. Diethylchlorophosphate (1.2 equivalents, 0.33 ml) which had been dissolved in dry DMF was added drop wise to this mixture and stirred for 12 hours at room temperature. The reaction mixture was quenched with water, extracted with ethyl acetate, the organic layer separated, washed with brine solution and dried over anhydrous sodium sulfate. The dried material was concentrated and purified by column chromatography to provide a pale yellow liquid (yield: 0.33 gram) and analyzed by HPLC (purity 93.1%). The FTIR, MS and 1H NMR spectra were consistent with the assigned with the empirical formula of C22H31N2O3P.
後処理
- additionwas added drop wise to this mixture
- customThe reaction mixture was quenched with water
- extractionextracted with ethyl acetate
- customthe organic layer separated
- washwashed with brine solution
- dry with materialdried over anhydrous sodium sulfate
- concentrationThe dried material was concentrated
- custompurified by column chromatography
出典と根拠
- ORDレコード
- ord-b1703efa99d34f4cba2f8ad87708452d
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08088918B2
関連ノート
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