反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of trans-2-(2-(6-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-2-methylpyrimidin-4-yl)cyclopropyl)benzo[d]thiazole (2-2) (26.0 mg, 72 μmol) in CH2Cl2 (0.2 mL) was added hydrochloric acid (4.0 M in 1,4-dioxane, 36.0 μL, 0.144 mmol, 2.0 eq.) and after 10 minutes the solvent was removed to afford trans-2-(2-(6-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-2-methylpyrimidin-4-yl)cyclopropyl)benzo[d]thiazole dihydrochloric acid salt (2-3) as an off-white solid. 1H NMR (300 MHz, DMSO-d6) δ 8.00 (br d, 1H, J=7.8 Hz), 7.89 (br d, 1H, J=7.8 Hz), 7.72 (s, 1H), 7.47 (td, 1H, J=7.8, 1.2 Hz), 7.38 (td, 1H, J=7.8, 1.2 Hz), 3.13 (ddd, 1H, J=8.7, 6.0, 4.0 Hz), 3.02 (ddd, 1H, J=8.7, 6.0, 4.0 Hz), 2.79 (s, 3H), 2.63 (s, 3H), 2.29 (s, 3H), 2.03-1.90 (m, 2H). LRMS m/z (M+H+) 363 found, 363 required. m.p. 194-195° C. dec.
WORKUP
后处理
- customafter 10 minutes the solvent was removed