反応 #162599

反応方程式

3-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-8-oxa-3-azabicyclo[3.2.1]octane

3-[6-Chloro-2-(4-nitro-phenyl)-pyrimidin-4-yl]-8-oxa-3-aza-bicyclo[3.2.1]octane

Sodium hydride

hydrogen

→

title compound

4-[4-Isopropoxy-6-(8-oxa-3-aza-bicyclo[3.2.1]oct-3-yl)-pyrimidin-2-yl]-phenylamine

溶媒

2-propanol

反応条件

後処理

1. 1
   その他to give a yellow suspension
2. 2
   その他to give a bright orange suspension
3. 3
   その他the solvents were evaporated
4. 4
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane
5. 5
   洗浄washed
6. 6
   乾燥The organic phase was dried over MgSO4
7. 7
   ろ過filtered
8. 8
   濃縮concentrated

実験手順

In a 2-5 mL microwave vial was placed 3-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-8-oxa-3-azabicyclo[3.2.1]octane (13, 70 mg, 0.202 mmol) in 2-propanol (4 mL) to give a yellow suspension. Sodium hydride (60% in oil, 32.3 mg, 0.807 mmol) was added and the mixture was stirred until no further formation of hydrogen gas was observed. The reaction was heated under microwave irradiation at 140° C. for 30 min to give a bright orange suspension. Work-up: the solvents were evaporated. The residue was dissolved in dichloromethane and washed with sat NaHCO3. The organic phase was dried over MgSO4, filtered and concentrated to give the title compound in a quantitative yield.

出典