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ChemicalBook CAS DataBase List 8-methoxy-3,4-dihydrobenzo[b]oxepin-5(2H)-one
98232-51-0

8-methoxy-3,4-dihydrobenzo[b]oxepin-5(2H)-one synthesis

6synthesis methods
-

Yield:98232-51-0 73%

Reaction Conditions:

with PPA in chlorobenzene at 80; for 15 h;

Steps:

19.C

The solution of PPA in chlor-benzene was added Compound Int-19d (22 g, 0.1 mol) at 80 °C and the mixture was allowed to stir at 80 °C for about 15 hours. The solution was removed and the residue was dissolved in ethyl acetate and washed with NaOH (IN, aqueous) followed by brine. The organic layer was dried over Na2S04, filtered and concentrated in vacuo to provide Compound Int-19e (14 g, 73 %). 1H NMR (CDC13) 6: 7.74 (d, J= 8 Hz, 1 H), 6.63 (d, J= 8 Hz, 1 H), 6.53 (s, 1 H), 4.21 (t, J= 12 Hz, 2 H), 3.80 (s, 3 H), 2.84 (t, J - 16 Hz, 2 H), 2.18 - 2.15 (m, 2H).

References:

WO2012/50848,2012,A1 Location in patent:Page/Page column 109-110

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