HRID2200038
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
A solution of (5-tert-butyl-2-methyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester (US 20040192653, 90 mg, 0.273 mmol), Intermediate 14e (150 mg, 0.273 mmol) and DIPEA (71 μL, 0.409 mmol) in dioxane (2 mL) was heated at 60° C. for 48 h. The reaction mixture was cooled and diluted with DCM (5 mL). The organic layer was washed with water (3×5 mL), passed through a phase separator and concentrated in vacuo. The residue was purified by FCC, using 0-10% [2M NH3 in MeOH] in DCM, to afford the title compound (117 mg, 59%). LCMS (Method 3): Rt: 5.12 min, m/z 729 [MH+].
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- washThe organic layer was washed with water (3×5 mL)
- concentrationconcentrated in vacuo
- customThe residue was purified by FCC