HRID1959385

反应详情

EQUATION

反应方程式

HRID 1959385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl N-tert-butoxycarbonyl-5-(4-(ethylsulfonyl)piperazin-1-yl)-3-((trimethylsilyl)ethynyl)pyrazin-2-ylcarbamate (589 mg, 1.037 mmol) was dissolved in anhydrous MeOH (10 mL) and treated with K2CO3 (14.33 mg, 0.1037 mmol). The reaction was allowed to stir at ambient temperature for 45 minutes. The solvent was removed in vacuo and the residue redissolved in DCM and washed with water followed by brine. The solution was dried (MgSO4), filtered and concentrated and the residue was purified by column chromatography (ISCO Companion™, 24 g column, 0-100% EtOAc/Petrol) to afford the title compound as an orange solid (287 mg, 60% Yield). 1H NMR (400.0 MHz, DMSO) d 1.23 (t, J=7.4 Hz, 3H), 1.38 (s, 18H), 3.11 (q, 2H), 3.26-3.34 (m, 4H), 3.69-3.71 (m, 4H), 4.65 (s, 1H) and 8.27 (s, 1H) ppm; MS (ES+) 396.0

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue redissolved in DCM
  3. washwashed with water
  4. dry with materialThe solution was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customthe residue was purified by column chromatography (ISCO Companion™, 24 g column, 0-100% EtOAc/Petrol)