HRID1685392

反应详情

EQUATION

反应方程式

HRID 1685392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of [5-(3,5-difluorophenyl)-5-methyl-2,4-dioxo-3-ethylimidazolidin-1-yl]acetic acid, isomer A (18 mg, 0.058 mmol, described in Intermediate 17), (R)-5-amino-1,3-dihydrospiro[indene-2,3′-pyrrolo[2,3-b]pyridin]-2′(1′H)-one (14 mg, 0.058 mmol, described in Intermediate 3), HOBT (13 mg, 0.086 mmol), EDC (17 mg, 0.086 mmol), and N,N-diisopropylethylamine (0.050 mL, 0.29 mmol) in DMF (0.5 mL) was stirred at 50° C. for 2 h. The reaction mixture was purified directly by HPLC using a reversed phase C18 column and eluting with a gradient of H2O:CH3CN:CF3CO2H—90:10:0.1 to 5:95:0.1. Lyophilization provided the title compound. MS: m/z=546 (M+1). HRMS: m/z=546.1944; calculated m/z=546.1948 for C29H26F2N5O4.

WORKUP

后处理

  1. customThe reaction mixture was purified directly by HPLC
  2. washeluting with a gradient of H2O