반응 #806642

반응 방정식

Di-imidazol-1-yl-methanone

2-ethyl-butan-1-ol

1-(4-methanesulfonyl-phenyl)-4-(piperidin-4-yloxy)-1H-pyrazolo[3,4-d]pyrimidine

triethylamine

→

solid

수율 44.6%

4-[1-(4-Methanesulfonyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy]-piperidine-1-carboxylic acid 2-ethyl-butyl ester

수율 44.6%

용매

DMSO

반응 조건

후처리

1. 1
   온도heated in a microwave at 120° C. for 6 minutes
2. 2
   기타The reaction mixture was quenched with water
3. 3
   추출the product was extracted with ethylacetate
4. 4
   기타Removal of organic solvents
5. 5
   기타in vacuo and purification by HPLC

실험 절차

Di-imidazol-1-yl-methanone (0.51 mmol, 83 mg), and 2-ethyl-butan-1-ol (0.51 mmol, 52 mg) were dissolved in DMSO (1 mL) and stirred for 30 minutes at room temperature. Then, 1-(4-methanesulfonyl-phenyl)-4-(piperidin-4-yloxy)-1H-pyrazolo[3,4-d]pyrimidine (0.17 mmol, 70 mg) and triethylamine (0.51 mmol, 72 μL) were added and heated in a microwave at 120° C. for 6 minutes. The progress of the reaction was monitored by LCMS. The reaction mixture was quenched with water and the product was extracted with ethylacetate. Removal of organic solvents in vacuo and purification by HPLC provided Compound A119 as a white solid (38 mg, 36%). Exact mass calculated for C24H31N5O5S 501.60, found 502.3 (MH+).

출처