HRID2216055

反应详情

EQUATION

反应方程式

HRID 2216055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{[4-(2′-Amino-4′-chloro-6′-methyl-biphenyl-3-sulfonyl)-5-methylsulfanyl-thiophen-2-yl]-imino-methyl}-carbamic acid tert-butyl ester (120 mg, 0.22 mmol, Example 135, e) and Et3N (0.91 μL, 0.65 mmol) were dissolved into DCM (4 mL). To this was added (4-Methanesulfonyl-butyryl chloride (0.144 M, 3.1 mL, 0.44 mmol, Example 209: a) and the reaction was stirred at RT overnight. The solvents were removed in vacuo followed by purification by flash column chromatography (20% EtOAc/hexanes) that yielded the title compound as an orange solid (124 mg, 81%). ESI-MS (m/z): Calcd. for C29H34ClN3O7S4: 700.1 (M+1) found: 700.1.

WORKUP

后处理

  1. customThe solvents were removed in vacuo
  2. customfollowed by purification by flash column chromatography (20% EtOAc/hexanes)