반응 #9741
ord-970f584521ce4e678ff7c29f9c38f8c9
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도with cooling for 3 hours
- 2추출the further water (50 ml), the resulting mixture was extracted twice with ethyl acetate
- 3건조dried over magnesium sulfate
- 4농축concentrated
- 5기타The residue was purified by SPE (Si cartridge)
- 6세척eluting initially with cyclohexane:chloroform (1:1)
실험 절차
A solution of ethyl 3-[(benzylthio)methyl]-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate (intermediate 45, 0.87 g) in dry tetrahydrofuran (5 ml) was cooled to 0° C. and 1M lithium aluminium hydride solution in diethyl, ether (0.299 ml) added. The reaction mixture as stirred with cooling for 3 hours. Water (0.5 ml) was added drop-wise followed by 2M hydrochloric acid (0.5 ml), the further water (50 ml), the resulting mixture was extracted twice with ethyl acetate, the extracts were combined, dried over magnesium sulfate and concentrated. The residue was purified by SPE (Si cartridge) eluting initially with cyclohexane:chloroform (1:1) and then chloroform to give the title compound as a white solid.