Tetrahydrofuran → 3-[(4-Chlorophenyl)sulfinyl]-N-[2-(diethylamino)ethyl]-1-pyrrolidinecarboxamide
反応式
[C:1](N1C=CN=C1)([N:3]1[CH:7]=[CH:6]N=C1)=[O:2].C(N[N:16]([CH2:20][CH3:21])NCC)C.[Cl:22][C:23]1[CH:28]=[CH:27][C:26]([S:29]([CH:31]2[CH2:35][CH2:34][NH:33][CH2:32]2)=[O:30])=[CH:25][CH:24]=1.O1CC[CH2:38][CH2:37]1>>[Cl:22][C:23]1[CH:24]=[CH:25][C:26]([S:29]([CH:31]2[CH2:35][CH2:34][N:33]([C:1]([NH:3][CH2:7][CH2:6][N:16]([CH2:20][CH3:21])[CH2:37][CH3:38])=[O:2])[CH2:32]2)=[O:30])=[CH:27][CH:28]=1参加物
5
実験手順
A solution of 4.37 g (0.027 mole) of 1,1'-carbonyldiimidazole and 2.96 g (0.0255 mole) of N,N-diethylaminoethylamine in 200 ml of tetrahydrofuran was stirred at room temperature for 45 min. A solution of 4.78 g (0.0209 mole) of 3-[(4-chlorophenyl)sulfinyl]pyrrolidine (free base) in tetrahydrofuran was added and the solution was refluxed for 16 hr. The solvent was removed in vacuo and the resulting oil was dissolved in methylene chloride. The methylene chloride solution was extracted with water and was dried over magnesium sulfate. The solvent was removed in vacuo. The solid residue was recrystallized from a mixture of methylene chloride, ether and hexane to give 3.45 g (44.4%) of white crystals, m.p. 127.5°-130° C.
後処理
- temperaturethe solution was refluxed for 16 hr
- customThe solvent was removed in vacuo
- dissolutionthe resulting oil was dissolved in methylene chloride
- extractionThe methylene chloride solution was extracted with water
- dry with materialwas dried over magnesium sulfate
- customThe solvent was removed in vacuo
- customThe solid residue was recrystallized from a mixture of methylene chloride, ether and hexane
出典と根拠
- ORDレコード
- ord-02cfb56102d44421b0edb76c45f43699
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04642348
反応ノート
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