反应详情

A solution of 70 mg product from Step A above, 38.1 mg EDC, 26.9 mg HOBt in 1 mL DMF was stirred at room temperature for 30 minutes. 5-Aminotetrazole monohydrate (20.5 mg) was added and the mixture stirred for additional 16 hours. Precipitate the product by adding 1 mL water to the reaction mixture. Collect the product by filtration, wash it with 1:1 DMF and water, water, and MeCN, and dry to give the title compound as a white solid. 1H NMR (CD3OD, 600 MHz) δ 7.92 (d, J=8.4 Hz, 2H), 7.42˜7.45 (m, 2H), 7.30 (d, J=8.2 Hz, 2H), 7.08 (d, J=8.4 Hz, 2H), 6.32 (s, 1H), 5.42 (s, 2H), 2.67 (tt, J=3.5 & 11.5 Hz, 1H), 1.97˜2.01 (m, 2H), 1.81˜1.85 (m, 2H), 1.72˜1.76 (m, 1H), 1.46˜1.53 (m, 2H), 1.38˜1.47 (m, 2H), 1.26˜1.35 (m, 1H). LC-MS: 2.30 min. (M+H=512.3).

1. customCollect the product
2. filtrationby filtration
3. washwash it with 1:1 DMF and water, water, and MeCN
4. customdry