Hydrochloric Acid → HCID 69592669, compound

Participants

Reaction Steps

The free base from Example 6 (8.7 g, 1 equiv) was dissolved in dichloromethane (50 ml) and 1M hydrogen chloride in ether (1 equiv) was added dropwise under argon. The mixture was evaporated to ca. half volume and sonicated to obtain a clear solution, which was transferred to a syringe and added dropwise to ether (200 ml) with vigorous stirring. The white solid was filtered off, washed with ether and dried in vacuo; yield 8.55 g. 1H-NMR (DMSO, ca 2:1 rotamer mixture) δ 1.14–1.24 (6H,m), 3.1 (6H, m), 3.6 (2H,m), 3.76 (3H,s), 4.38/4.45 (2H,2x s), 4.61/4.70 (2H,2x s), 4.98/5.11 (2H,2x s), 6.75/6.79 (1H,2x s), 7.1–7.7 (15H,m), 10.15/10.75 (1H,2x br s; MS (APCI+) found (M+1)=687/689; C37H40ClFN6O2S requires 686/688.

Provenance & Evidence