HRID489700

反应详情

EQUATION

反应方程式

HRID 489700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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-oxo-2-[4-(2-{[(2,4,6-trimethylphenyl)sulfonyl]amino}phenyl) piperidyl]ethyl)carbamoyl)(3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step a) (146 mg, 0.18 mmol) and 50% TFA in CH2Cl2 (10 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 (TFA salt) as a white foam (81 mg). MS (ESI, pos. ion) m/z: 699 (M+1); (ESI, neg. ion) m/z: 697 (M−1). Calc'd for C30H43ClN4O4S: 698.27.

WORKUP

后处理

  1. customThe title compound was prepared
  2. customPurification by reverse phase preparative HPLC [Phenomenex