反応 #8682

反応方程式

water

sodium carbonate

3-[5-(2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine

2-iodopropane

→

1-(2-Fluorobenzyl)-3-[5-(5-isopropyl-2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1H-pyrazol[3,4-b]pyridine

溶媒

acetone

反応条件

後処理

1. 1
   抽出extracted with DCM
2. 2
   洗浄washed with saturated aqueous sodium chloride solution
3. 3
   その他dried
4. 4
   ろ過filtered
5. 5
   その他The solvent is removed in vacuo
6. 6
   その他the residue is purified by preparative HPLC with addition of small portions of aqueous hydrochloric acid
7. 7
   その他25 mg (42% of theory) of the product are obtained

実験手順

50 mg (0.13 mmol) of 3-[5-(2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine (example 9) are dissolved in 5 ml of absolute acetone, and 92 mg (0.87 mmol) of sodium carbonate are added. 64 mg (0.37 mmol) of 2-iodopropane are added to the suspension, and the mixture is stirred at RT overnight. The reaction solution is mixed with water and extracted with DCM. The organic phases are combined, washed with saturated aqueous sodium chloride solution, dried and filtered. The solvent is removed in vacuo, and the residue is purified by preparative HPLC with addition of small portions of aqueous hydrochloric acid. 25 mg (42% of theory) of the product are obtained.

出典