Cesium carbonate → 2-(4-Bromophenyl)-1lambda~6~,2-thiazolidine-1,1-dione
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:9]([CH2:12][CH2:13][CH2:14]Cl)(=[O:11])=[O:10])=[CH:4][CH:3]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.CCOCC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][S:9]2(=[O:11])=[O:10])=[CH:4][CH:3]=1参加物
5
実験手順
N-(4-Bromophenyl)-3-chloropropane-1-sulfonamide (1.0 g, 3.2 mmol) was dissolved in DMF, Cs2CO3 (1.56 g, 4.8 mmol) was added, and the mixture was stirred for 3 hours. The mixture was then diluted with ether, washed with water, 2N HCl, brine, dried over MgSO4, and concentrated. The crude product was purified via Isco chromatography (the Redisep® column, silica, gradient 5-60% ethyl acetate in hexane) to afford 0.65 g (74%) 2-(4-bromophenyl)isothiazolidine 1,1-dioxide.
後処理
- washwashed with water, 2N HCl, brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe crude product was purified via Isco chromatography (the Redisep® column, silica, gradient 5-60% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-badd3839ed964d90b8c6c5b71323ed65
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07291643B2
反応ノート
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