反应 #1857597

反应方程式

hydroxybenzotriazole

Trisamine

1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride

Hydroxybenzotriazole

benzo[d][1,3]dioxole-5-carboxylic acid

→

desired product

收率 6.0%

N-(1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-yl)benzo[d][1,3]dioxole-5-carboxamide

收率 6.0%

溶剂

dimethylformamide

Acetonitrile

dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONwas added into the reaction well
2. 2
   workup.ADDITIONwas added into the reaction mixture
3. 3
   workup.WAITto shake overnight at room temperature
4. 4
   workup.STIRRINGshaken for 1 minute
5. 5
   其他The solution was evaporated under vacuum

实验过程

1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride (example 1a) (8 mg, 35 μmol) and benzo[d][1,3]dioxole-5-carboxylic acid (7 mg, 42 μmol) were each dissolved in 200 uL dimethylformamide. Si-Carbodiimide resin (70 mg, 70 μmol) was loaded into a 1.2 mL 96 well Greiner plate, followed by the addition of amine and acid. Hydroxybenzotriazole (6 mg, 42 μmol) was dissolved in 100 uL dimethylformamide and was added into the reaction well. The reaction was shaken overnight at room temperature. To remove excess carboxylic acid and hydroxybenzotriazole, PS-Trisamine resin (35 mg, 70 μmol) was added into the reaction mixture and was allowed to shake overnight at room temperature. 200 uL of Acetonitrile was added into the reaction well and shaken for 1 minute. The top clear solution was transferred into a new plate. The extraction process was repeated two more times. The solution was evaporated under vacuum and gave the desired product. Yield 6%. MS M+H calculated 341.1. Found 341.2.

来源