HCID 68953639, compound → HCID 16041821, compound

Participants

Reaction Steps

A product obtained in Example 2 (0.1 g, 0.27 ml) was dissolved in pyridine (10 ml), adding acetyl anhydride (0.5 ml). The mixture was stirred at room temperature for 2 hours. The mixture was concentrated under reduced pressure and added water. Then the aqueous phase was adjust to pH 8 with saturated NaHCO3 and extracted with CH2Cl2. The combined organic layers were washed with brine and dried over Na2SO4, filtered, and the solvent was evaporated under reduced pressure to give pale desired product (0.073 g, 64.6%). mp 212˜214° C. 1HNMR (CDCl3) δ: 2.33 (3H, s, COCH3), 2.34 (3H, s, COCH3), 2.63˜2.75 (3H, m, CH2), 3.13˜3.20 (3H, m, CH2), 3.41˜3.56 (2H, m, CH2 and N—CH), 3.81 (3H, s, Ar—OCH3), 3.82 (3H, s, Ar—OCH3), 4.02 (1H, d, CH2), 6.70 (1H, s, ArH), 6.83 (1H, d, ArH), 6.92 (1H, s, ArH), 7.00 (1H, s, ArH).

Provenance & Evidence