반응 #45120
ord-fc3dbbd8a23444f3b8066829388d5400
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반응물
시약
반응 조건
후처리
- 1여과the mixture was filtered through celite
- 2기타The filtrate was transferred to a separating funnel
- 3기타the aqueous layer removed
- 4세척The ethyl acetate layer was washed with saturated brine
- 5건조dried over magnesium sulphate
- 6여과After filtration the solvent
- 7기타was evaporated
- 8기타to give the crude product as a yellow gum
- 9기타The crude product was purified by preparative LCMS
- 10workup.ADDITIONFractions containing the desired compound
- 11기타were evaporated to dryness
실험 절차
2M Trimethylaluminium (1.250 ml, 2.50 mmol) in toluene, was added dropwise to a stirred solution of ethyl 5-(3,3-dimethylpiperazin-1-yl)thiophene-2-carboxylate (0.268 g, 1 mmol) and 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine hydrochloride (0.286 g, 1.00 mmol) in toluene (7.14 ml) at 65° C. under nitrogen. The reaction mixture was stirred and heated at 65° C. for 4 h then 50° C. for 18 h followed by 80° C. for 5 h. Ethyl acetate (5 mL) was added to the reaction mixture followed by a solution of potassium sodium tartrate (5 mL, 20% aqueous). More ethyl acetate (50 mL) and water (25 mL) was added and the mixture was filtered through celite. The filtrate was transferred to a separating funnel and the aqueous layer removed. The ethyl acetate layer was washed with saturated brine and then dried over magnesium sulphate. After filtration the solvent was evaporated to give the crude product as a yellow gum. The crude product was purified by preparative LCMS, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the title compound (0.073 g, 15.48%) as a white solid.