[OH:1]OS([O-])=O.[K+].C(N([CH2:23][C:24]([OH:26])=O)CC(O)=O)CN(CC(O)=O)CC(O)=O.[CH3:27][C:28]1[CH:29]=[C:30]([C:33](=O)[CH3:34])[S:31][CH:32]=1.S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+].[OH2:45]>CC(C)=O>[CH3:32][S:31]([C:30]1[CH:33]=[CH:34][C:27]([C:24](=[O:26])[CH3:23])=[CH:28][CH:29]=1)(=[O:1])=[O:45]
A solution of 1036 g of oxone and 11.7 g of EDTA (Ethylene diamine tetraacetic acid) dissolved in 3.8 l of water is added dropwise to a solution of (4-methylthiophenyl)ethanone (prepared according to J. Am. Chem. Soc. 1952 p. 5475) in 1 l of acetone and 1.1 l of water, the temperature being kept below 32° C. The reaction mixture is stirred for 16 h after the end of the addition, then 550 g of sodium metabisulphite are added portionwise. The reaction mixture is then filtered, the solid obtained is taken up in water, dried in the oven and recrystallised from ethanol.
読み込み中…
