HRID2216156

反应详情

EQUATION

反应方程式

HRID 2216156 的结构方程式

PROCEDURE

实验过程

({4-[6′-(2-bromo-acetylamino)-2′-methyl-biphenyl-3-sulfonyl]-5-methylsulfanyl-thiophen-2-yl}-imino-methyl)-carbamic acid tert-butyl ester (22 mg, 0.034 mmol, as prepared in Example 246, step a) was stirred in a mixture of TFA/DCM (1:1, 4 mL) for 1 h at rt. The reaction was concentrated in vacuo and the resulting residue was purified using RP-HPLC (10–50% CH3CN in H2O with 0.1% TFA over 30 min) to afford 15 mg (68%) of the title compound as a clear glassy solid (purity>99.9% by analytical RP-HPLC). ESI-MS (m/z): Calcd. for C21H20BrN3O3S3: 538.0 (M+H); found: 538.0 and 540.0

WORKUP

后处理

  1. concentrationThe reaction was concentrated in vacuo
  2. customthe resulting residue was purified
  3. customRP-HPLC (10–50% CH3CN in H2O with 0.1% TFA over 30 min)