反应详情

316 mg (0.83 mmol) of 4-(5-methoxymethyl-5-methyl-2,3,4,5-tetrahydrobenzo[b]thiepin-8-ylethynyl)-benzoic acid methyl ester was dissolved in 8 ml of THF/EtOH (1/1) and treated with 1.38 ml of 3N NaOH (5 eq.). The reaction flask was kept in the dark and stirring continued for 18 h at room temperature. The mixture was then poured onto crushed ice/ HCl, extracted twice with diethylether, the organic phase was washed with brine, dried over magnesium sulfate, filtrated and evaporated to dryness. Crystallization of the residue from hexane/ethylacetate yielded 282 mg of the title product as white crystals of m.p. 182-183° C.

1. additionThe mixture was then poured
2. extractionextracted twice with diethylether
3. washthe organic phase was washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltrated
6. customevaporated to dryness
7. customCrystallization of the residue from hexane/ethylacetate