HRID1926347
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 5-(3-aminoprop-1-ynyl)-3-benzothiazol-2-ylpyridin-2-ylamine (10.0 mg, 0.0357 mmol), trimethylsilyl isocyanate (5.31 uL, 0.0392 mmol), DMF (1 mL, 0.01 mol) and DIPEA (0.03 mL, 0.2 mmol) was stirred at rt for 3 h. The solution was used directly for HPLC purification. The fractions containing the pure product were concentrated in vacuo to afford the title compound as a yellow solid. 1H NMR (400 MHz, CD3OD): δ=4.14 (s, 2H), 7.39-7.45 (m, 1H), 7.47-7.52 (m, 1H), 7.93 (s, 1H), 8.00 (d, J=7.8 Hz, 1H), 8.06 (d, J=2.0 Hz, 1H). MS (ES+): m/z=324.10 (100) [MH+]. HPLC: tR=2.85 min (ZQ3, polar—5 min).
WORKUP
后处理
- customThe solution was used directly for HPLC purification
- additionThe fractions containing the pure product
- concentrationwere concentrated in vacuo