تفاعل #45141
ord-04ef702d9aa349aa9a295d641b6c2474
معادلة التفاعل
المتفاعلات
الكواشف
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المعالجة
- 1درجة الحرارةThe reaction mixture was cooled
- 2أخرىquenched with methanol (15 ml) and 2N hydrochloric acid (5 ml)
- 3أخرىThe crude reaction mixture
- 4أخرىwas purified by ion exchange chromatography on a SCX column
- 5غسيلeluting with 7N ammonia in methanol
- 6أخرىThe appropriate fractions were evaporated
- 7أخرىto give an oil
- 8أخرىThe crude product was purified by silica column chromatography
- 9غسيلeluting with a gradient of 0 to 10% 2.5N ammonia/MeOH in DCM
- 10أخرىPure fractions were evaporated to dryness
- 11أخرىto afford, on crystallisation from DCM/diethyl ether
الإجراء التجريبي
A 2M solution of trimethylaluminium (2.500 mL, 5.00 mmol) in toluene, was added dropwise to a stirred suspension of ethyl 4-((3R,5S)-3,4,5-trimethylpiperazin-1-yl)benzoate (0.643 g, 2 mmol) and 5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-amine (0.495 g, 2.00 mmol) in toluene (10 mL) at room temperature. The solution was then heated at 60° C. for 18 h. The reaction mixture was cooled and quenched with methanol (15 ml) and 2N hydrochloric acid (5 ml). The crude reaction mixture was purified by ion exchange chromatography on a SCX column, eluting with 7N ammonia in methanol. The appropriate fractions were evaporated to give an oil. The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 10% 2.5N ammonia/MeOH in DCM. Pure fractions were evaporated to dryness to afford, on crystallisation from DCM/diethyl ether, the title compound (0.322 g, 33.7%) as a cream solid.