反应详情

A mixture of 3.60 g (11.73 mmol) of 1-(4-chlorophenyl)-6-(tetrahydro-2H-pyran-2-yloxy)hex-2-yn-1-one, prepared in stage 5.2., of 9.45 g (117 mmol) of formamidine hydrochloride and of 25 g (234 mmol) of sodium carbonate in suspension in 108 ml of acetonitrile and 0.1 ml of water is stirred at 40° C. for 5 hours. The mixture is subsequently taken up in 600 ml of water and 400 ml of a saturated aqueous sodium carbonate solution. The organic phase is separated by settling, washed with 200 ml of water and 200 ml of a saturated aqueous sodium chloride solution, dried over sodium sulphate and evaporated. The residue is purified by chromatography on silica gel, elution being carried out with a 70/30 mixture of n-hexane and of ethyl acetate, to produce 3.22 g (9.67 mmol) of product in the form of a yellowish oil.

1. customprepared in stage 5.2
2. customThe organic phase is separated
3. washwashed with 200 ml of water and 200 ml of a saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulphate
5. customevaporated
6. customThe residue is purified by chromatography on silica gel, elution
7. additionbeing carried out with a 70/30 mixture of n-hexane and of ethyl acetate