反応式
[CH3:1][S:2]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:4])=[O:3].C(=O)([O-])[O-].[K+].[K+].Br[CH2:18][CH2:19][Cl:20]>C(#N)C>[Cl:20][CH2:19][CH2:18][N:8]1[CH2:9][CH2:10][N:5]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:6][CH2:7]1参加物
5
実験手順
A mixture of 1-(methylsulfonyl)piperazine (250 mg, 1.522 mmol), potassium carbonate (1262 mg, 9.13 mmol) and 1-bromo-2-chloroethane (1092 mg, 7.61 mmol) in acetonitrile (5 mL) was stirred for 6 hours at room temperature. LCMS indicated the formation of desired product. The reaction mixture was filtered to remove the white precipitate, then quenched with distilled water (10 mL), extracted with ethyl acetate (3×8 mL), the extracts were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the clean desired product as white solid (100 mg, 29%). LCMS: m/e 227.15 (M+H)+, 1.21 min (method 10).
出典と根拠
- ORDレコード
- ord-19ad2a3a85a444e3ba8bdb52476b5267
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846647B2
関連ノート
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