HRID1799109

反应详情

EQUATION

反应方程式

HRID 1799109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 5-(3-methoxyprop-1-ynyl)-2-phenylthiazole-4-carboxylate (26.1 g, 86.6 mmol) was dissolved in EtOAc (350 mL) and hydrogenated under balloon pressure for four days until LCMS indicated complete reduction of unsaturation. On day three, the catalyst was removed by filtration, fresh catalyst added and the mixtures re-subjected to hydrogenation at balloon pressure. The catalyst was removed by filtration through a pad of celite. The filter pad was rinsed with EtOAc and the filtrate concentrated to dryness. The crude product was purified by MPLC eluting with pentane/EtOAc to give ethyl 5-(3-methoxypropyl)-2-phenylthiazole-4-carboxylate (23.2 g, 88% yield).

WORKUP

后处理

  1. waitOn day three
  2. customthe catalyst was removed by filtration, fresh catalyst
  3. additionadded
  4. customThe catalyst was removed by filtration through a pad of celite
  5. washThe filter pad was rinsed with EtOAc
  6. concentrationthe filtrate concentrated to dryness
  7. customThe crude product was purified by MPLC
  8. washeluting with pentane/EtOAc