반응 #416585
ord-82d4d90b35544a80aca467bfe97325ee
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타To a 125 ml round-bottomed flask equipped with condenser and N2 inlet
- 2온도The reaction was heated
- 3온도at reflux for 5 days
- 4온도cooled
- 5여과the precipitate filtered
- 6세척washed with sodium bicarbonate
- 7건조dried over sodium sulfate
- 8workup.ADDITIONtreated with methylene chloride saturated with hydrochloride
- 9기타evaporated
- 10기타the residue triturated with ether
- 11기타to afford a white solid, m.p. 305°-307° C., 1.76 g (48%)
실험 절차
To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 1.59 g (7.5 mmol) of N-(1-naphthyl)piperazine, 1.31 ml (7.5 mmol) of diisopropylethylamine, 1.59 g (15 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered. The solid was taken up in methylene chloride, washed with sodium bicarbonate, dried over sodium sulfate, treated with methylene chloride saturated with hydrochloride, evaporated, and the residue triturated with ether to afford a white solid, m.p. 305°-307° C., 1.76 g (48%).