HRID595107

反应详情

EQUATION

反应方程式

HRID 595107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of methyl 6-[bis-(tert-butoxycarbonyl)amino]-3-[2-(tetrahydropyran-2-yl)-2H-pyrazol-3-yl]-2-vinylbenzoate (Intermediate 10, 2.6 g) and concentrated hydrochloric acid (3 drops) in methanol (80 mL) was stirred at room temperature for 30 minutes. The solution was treated with saturated aqueous sodium bicarbonate solution and the mixture was concentrated in vacuo. The residue was partitioned between ethyl acetate and water and the organic layer was dried (MgSO4) and filtered. The filtrate was concentrated in vacuo to give methyl 6-[bis-(tert-butoxycarbonyl)amino]-3-(2H-pyrazol-3-yl)-2-vinylbenzoate (2.38 g) as a white solid.

WORKUP

后处理

  1. concentrationthe mixture was concentrated in vacuo
  2. customThe residue was partitioned between ethyl acetate and water
  3. dry with materialthe organic layer was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo