1-Hydroxybenzotriazole → HCID 178522661, compound

Participants

Reaction Steps

A mixture of 44.4 mg product from Step B above, 28.8 mg EDC, 20.3 mg HOBt and 13.4 mg aminotetrazole monohydrate was dissolved in 1 mL DMF. DIEA (44 μL) was added immediately and the resulting solution was stirred at room temperature for five days. The reaction mixture was diluted with a mixture of DMF, MeCN, 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 (CD3OD, 500 MHz) δ 8.03 (d, J=8.3 Hz, 2H), 7.84˜7.86 (m, 2H), 7.46 (d, J=8.2 Hz, 2H), 7.28 (d, J=8.2 Hz, 2H), 6.47 (s, 1H), 4.23 (s, 2H), 4.055 (tt, J=3.7 & 11.7 Hz, 1H), 1.88˜1.97 (m, 2H), 1.81˜1.85 (m, 2H), 1.67˜1.73 (m, 3H), 1.25˜1.39 (m, 3H). LC-MS: 2.34 min. (M+H=512.2).

Provenance & Evidence