1-Hydroxybenzotriazole → HCID 178522663, compound

Participants

Reaction Steps

A mixture of 66.7 mg product from Step B above, 71.9 mg EDC, 30.4 mg HOBt and 23.2 mg aminotetrazole monohydrate was dissolved in 1 mL DMF. DIEA (92 μL) was added immediately and the resulting solution was stirred at room temperature for 17 hours. The reaction mixture was diluted with about 2:1 mixture of DMF and water and purified on preparative HPLC using 70˜80% MeCN gradient over 10 minutes at 8.0 mL per minute with 0.1% TFA. The title compound was obtained as a white solid following lyophilization. 1H NMR (DMSO-d6, 500 MHz) δ 8.26 (s, 1H), 8.02 (d, J=8.2 Hz, 2H), 7.84˜7.87 (m, 2H), 7.40˜7.45 (m, 4H), 3.92 (s, 2H), 2.58 (tt, J=3.4 & 11.9 Hz, 1H), 1.62˜1.74 (m, 5H), 1.41˜1.50 (m, 2H), 1.17˜1.31 (m, 3H). LC-MS: 2.41 min. (M+H=512.3).

Provenance & Evidence