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
The title compound was prepared according to the procedure described in Example 3 (Step b) using tert-butyl 3-[N-((1R)-1-[(4-chlorophenyl)methyl]-2-(4-[2-(methoxycarbonylamino)-phenyl]-piperidyl}-2-oxoethyl)-carbamoyl](3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step a) (412 mg, 0.61 mmol) and 50% TFA in CH2Cl2 (20 mL). Purification by reverse phase preparative HPLC [Phenomenex; 5 μm 250×21.2 mm, 5% to 95% CH3CN (0.1% TFA) in H2O (0.1% TFA) over 30 min, then 100% CH3CN (0.1% TFA) for 2 min] provided the title compound as a white foam (159 mg). MS (ESI, pos. ion) m/z: 575 (M+1); (ESI, neg. ion) m/z: 573 (M−1). Calc'd for C32H35ClN4O4: 574.23. Anal. Calcd for C32H35ClN4O4.18C2HF3O2: C, 57.45; H, 5.06; N, 7.75. Found: C, 57.66; H, 5.09; N, 7.62.
WORKUP
后处理
- customThe title compound was prepared
- customPurification by reverse phase preparative HPLC [Phenomenex