Diethyl Ether → HCID 10973591, compound

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Reaction Steps

2-(4-Chloro-5-dimethylamino-2-nitro-phenylsulfanyl)-N,N-dimethyl-benzamide (22) (0.5 g, 1.32 mmol) and methyl trifluoromethanesulfonate (0.3 g, 1.83 mmol) was heated to reflux in 5 mL of methylene chloride for 72 h. After cooled down, ethyl ether was added to the mixture. Precipitate was collected and recrystalized from CH2Cl2/ethylether repeatedly. Highly hygroscopic pale yellow powder was dried in vacuo and used directly for F-18 radiolabeling without further purifications (Yellow powder. 0.31 g, 40%): IR (cm−, neat) 3060, 1623, 1553, 1519, 1256, 1154, 1027, 784, 640; 1H NMR (200 MHz CDCl3) δ 8.53 (s, 1H), 7.74–7.90 (m, 4H), 7.69 (s, 1H), 3.69 (s, 9H), 3.40 (s, 3H), 3.06 (s, 3H); HRMS calcd for C18H2135ClN3O3S (M+) 394.0992, found 394.0999.

Provenance & Evidence