Sodium methanesulfinate → HCID 86697221、化合物

反応式

[CH3:1][S:2]([O-:4])=[O:3].[Na+].CS(O[CH2:11][C:12]([CH3:25])([CH3:24])[CH2:13][O:14][C:15]1[CH:20]=[C:19]([CH3:21])[C:18]([Br:22])=[C:17]([CH3:23])[CH:16]=1)(=O)=O>CN1CCCC1=O.C(OCC)C>[Br:22][C:18]1[C:17]([CH3:23])=[CH:16][C:15]([O:14][CH2:13][C:12]([CH3:25])([CH3:24])[CH2:11][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:20][C:19]=1[CH3:21]

参加物

反応条件

温度: 180 °C

実験手順

In a microwave vial sodium methanesulfinate (720 mg) is added to a solution of 3-(4-bromo-3,5-dimethylphenoxy)-2,2-dimethylpropyl methanesulfonate (271 mg) in N-methyl-2-pyrrolidinon (NMP) (8 mL). The mixture is heated to 180° C. for 30 minutes. Then the mixture is diluted with diethylether, washed with water and brine and dried (MgSO4). The solvent is evaporated and the residue is purified by HPLC on reversed phase to give the title compound. Yield: 32 mg; LC (method 8): tR=0.47 min; Mass spectrum (ESI+): m/z=349 [M+H]+.