Chlorosulfonic acid → HCID 9850567, compound

Participants

Reaction Steps

A solution of 10 (0.20 g, 0.42 mmol) in CH2Cl2 (100 mL) at about 0° C. was treated with chlorosulfonic acid (0.056 g, 1.1 eq) and stirred for about 2 h. The reaction was Warmed to about rt, stirred for about 18 h and evaporated to a tan powder. The powder was purified by preparative HPLC (MeCN:water, 1:3) to give 18 (tan powder). 1H NMR (DMSO-d6) 2.1 (m, 4 H), 3.0 (m, 1 H), 3.2 (t, J=4, 1 H), 6.1 (m, 1 H), 6.7 (t, J=6, 1 H), 6.9 (d, J=5, 1 H), 7.1 (m, 4 H), 7.3-7.6 (m, 9 H), 10.3 (br. s, 2 H), 11.1 (s, 1 H). MS m/e 552.62 (MH+).

Provenance & Evidence