反応 #166307

反応方程式

compound 4

9-Cyclopentyl-9H-pyrido[4′,3′:4,5]pyrrolo[2,3-d]pyrimidin-2-amine

3,6-dichloropyridazine

Xantphos

sodium tert-butoxide

→

compound 140

収率 97.0%

6-((9-cyclopentyl-9H-pyrido[4′,3′:4,5]pyrrolo[2,3-d]pyrimidin-2-yl)amino)-3-chloro-pyridazine

収率 97.0%

溶媒

toluene

反応条件

後処理

1. 1
   その他was purged with nitrogen
2. 2
   温度After cooling to room temperature
3. 3
   洗浄eluted with 2-10% methanol/DCM
4. 4
   その他Evaporation of combined fractions

実験手順

A mixture of compound 4 (1.50 g, 5.92 mmol), 3,6-dichloropyridazine (0.882 g, 5.92 mmol), bis(dibenzylideneacetone)palladium (0.170 g, 0.296 mmol), Xantphos (0.514 g, 0.888 mmol) and sodium tert-butoxide (0.854, 8.88 mmol) in toluene (80 mL) was purged with nitrogen. The reaction was then heated at 100° C. for one hour in a sealed vessel. After cooling to room temperature, the mixture was loaded onto a silica gel column and eluted with 2-10% methanol/DCM. Evaporation of combined fractions provided compound 140 (2.1 g) as a yellowish solid. LCMS-ESI, M+1: 366.1

出典