HRID549238

反应详情

EQUATION

反应方程式

HRID 549238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (4.06 g, 21.2 mmol) was added to a solution of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxylic acid (4.88 g, 19.3 mmol) and 1-hydroxybenzotriazole (2.87 g, 21.2 mmol) in N,N-dimethylformamide (DMF) (24.4 mL) at room temperature. The mixture was stirred for two hours, cooled in an ice bath, and treated with concentrated ammonium hydroxide (3.9 mL). A precipitate formed, and the mixture was stirred 30 minutes at 0° C. Water (100 mL) was added, and the mixture was stirred for an additional ten minutes. The precipitate was isolated by filtration, washed with water, and dried on the vacuum filter funnel to provide 4.05 g of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxamide as white crystals.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customA precipitate formed
  3. stirringthe mixture was stirred 30 minutes at 0° C
  4. stirringthe mixture was stirred for an additional ten minutes
  5. customThe precipitate was isolated by filtration
  6. washwashed with water
  7. customdried on the vacuum
  8. filtrationfilter funnel