NCc1ccccc1.O=C1NCCc2cc(Br)ccc21>CC(=O)O.CC(=O)O.CC(C)(C)[O-].CN(C)C=O.[K+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>O=C1NCCc2cc(NCc3ccccc3)ccc21
**Repeat 02915-84 but use MW* only. Reduce benzylamine from 4 to 2 eqs.** In a 10 mL sealed MW* test tube was 6-bromo-3,4-dihydroisoquinolin-1(2H)-one (100 mg, 0.44 mmol), phenylmethanamine (97 µl, 0.88 mmol), BINAP (13.77 mg, 0.02 mmol) and palladium(II) acetate (4.97 mg, 0.02 mmol) in DMF (500 mL) combined to give a tan suspension. potassium tert-butoxide (49.6 mg, 0.44 mmol) was then added last. Placed test tube onto Smith MW* platform. Heated reaction to 130°C for 15 minutes. Reaction know a cloudy pale amber. Took LCMS - there is NO product present, ALL SM!!! Placed sealed test tube in heated (130°C) oil bath over weekend. Took LCMS - all SM is consumed but NO desired product is seen!!! Discarded reaction.
Loading…
