Triethylamine → 1-(2-Acetylaminoethyl)-2,5-dimethyl-3-methylsulphinylpyrrole
反応式
[CH3:1][S:2](Cl)=[O:3].[C:5]([NH:8][CH2:9][CH2:10][N:11]1[C:15]([CH3:16])=[CH:14][CH:13]=[C:12]1[CH3:17])(=[O:7])[CH3:6].C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[C:5]([NH:8][CH2:9][CH2:10][N:11]1[C:12]([CH3:17])=[CH:13][C:14]([S:2]([CH3:1])=[O:3])=[C:15]1[CH3:16])(=[O:7])[CH3:6]参加物
6
反応条件
- 温度
- 0 °C
実験手順
19.7 g (0.2 mol) of methylsulphinyl chloride are dissolved in 500 ml of methylene chloride. 36.0 g (0.2 mol) of 1-(2-acetylaminoethyl)-2,5-dimethylpyrrole and 27.6 ml (0.2 mol) of triethylamine in 500 ml of methylene chloride are added dropwise at 0° C. and the mixture is stirred at 0° C. for 45 minutes and poured onto aqueous sodium bicarbonate solution. The organic phase is separated off and discarded. The aqueous phase is concentrated and the residue is boiled up with isopropanol and, after the mixture has been concentrated, the product is chromatographed.
後処理
- customThe organic phase is separated off
- concentrationThe aqueous phase is concentrated
- concentrationafter the mixture has been concentrated
- customthe product is chromatographed
出典と根拠
- ORDレコード
- ord-4f539bc04d6443cdaa8a93904c4f8384
- 出典データセット
- uspto-grants-1990_10
- 特許番号
- US04966901
反応ノート
読み込み中…