HRID2409101

反应详情

EQUATION

反应方程式

HRID 2409101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 100 mL round bottom flask equipped with a stir bar was added 0.964 g of methyl 5-(5-chloro-4-(methylamino)pyrimidin-2-ylamino)-1-methyl-1H-pyrazole-3-carboxylate, 0.28 g of LiOH, 15 mL of tetrahydrofuran and 10 mL of water. The reaction was stirred at room temperature for 18 hours. The tetrahydrofuran was removed in vacuo and the aqueous layer was acidified to pH 5 with 1N HCl. The aqueous layer was partitioned with ethyl acetate and the organic layer washed with brine, dried over MgSO4, filtered and concentrated to give 0.58 g of 5-(5-chloro-4-(methylamino)pyrimidin-2-ylamino)-1-methyl-1H-pyrazole-3-carboxylic acid which was used without further purification.

WORKUP

后处理

  1. customTo a 100 mL round bottom flask equipped with a stir bar
  2. customThe tetrahydrofuran was removed in vacuo
  3. customThe aqueous layer was partitioned with ethyl acetate
  4. washthe organic layer washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated