Hydrochloric Acid → HCID 71082612, compound

Participants

Reaction Conditions

Reaction Steps

65 mg of (S)-methyl 2-(2-pivaloyloxy-6,7-dihydrothieno[3,2-c]pyridin-5(4H)-yl)-2-(2-chlorophenyl)-acetate (I-7) was dissolved in 4 ml of diethyl ether, and stirred in an ice-salt bath at −10° C. A hydrogen chloride saturated ethanol solution (0.2 ml) was added slowly dropwise, till the system reached about pH 2, at which a white solid was precipitated immediately. It was stirred for 5 min, allowed to stand, quickly filtered under a nitrogen atmosphere, and washed with a suitable amount of diethyl ether. The resulting solid was dried in vacuum to obtain the I-7 hydrochloride (65 mg, granular solid). Yield: 92%, melting point: 135-137° C.; 1H-NMR (300 MHz, CDCl3) δ 1.33 (s, 9H), 3.08 (s, 2H), 3.44-3.51 (m, 2H), 3.82 (s, 4H), 4.34 (s, 1H), 5.59 (s, 1H), 6.39 (s, 1H), 7.44-7.50 (m, 3H), 8.36 (d, 1H, J=7.2 Hz).

Provenance & Evidence