Sodium hydride → Diallyl 2,2-bis(pyrenylmethyl)malonate

関与物質

反応手順

Diallyl malonate (0.36 g, 2.0 mmol) was added to a stirred suspension of NaH (2.5 mmol) in dry benzene (5 mL). After 30 minutes 1-chloromethylpyrene (0.5 g, 2.0 mmol) in benzene (20 mL) was added. The mixture was gently refluxed for 18 hours, cooled to room temperature and washed with saturated aqueous NaCl (2×5 mL). The organic layer was dried over MgSO4 and the solvent evaporated under reduced pressure to give the product, which was recrystallized from AcOEt/hexane to afford the desired product as white crystals, yield: 0.26 g, 42%, m.p. 178°-180° C. 1H NMR and 13C NMR were in accord with the desired product. Analysis (C43H32O4): calculated C:84.29, H:5.26; found: C:84.13, H:5.23.

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