反応 #162606

反応方程式

4-(8-oxa-3-azabicyclo[3.2.1]octan-3-yl)-6-chloropyrimidin-2-ol

4-(8-Oxa-3-azabicyclo[3.2.1]octan-3-yl)-6-chloropyrimidin-2-ol

8-Oxa-3-azabicyclo[3.2.1]octane, HCl

8-oxa-3-aza-bicyclo[3.2.1]octane hydrochloride

DIPEA

→

title compound

収率 42.0%

4,6-Di(8-oxa-3-azabicyclo[3.2.1]octan-3-yl)pyrimidin-2-ol

収率 42.0%

溶媒

MeOH

反応条件

後処理

1. 1
   その他to give a colorless solution
2. 2
   workup.ADDITIONSilica gel was added
3. 3
   その他the solvents were removed under reduced pressure
4. 4
   その他The mixture was purified by HPLC

実験手順

In a 2-5 mL microwave vial was placed 4-(8-oxa-3-azabicyclo[3.2.1]octan-3-yl)-6-chloropyrimidin-2-ol (26, 50 mg, 0.207 mmol) in MeOH (2.5 ml) to give a colorless solution. 8-Oxa-3-azabicyclo[3.2.1]octane, HCl (2, 61.9 mg, 0.414 mmol) and DIPEA (0.217 ml, 1.241 mmol) were added. The reaction was heated under microwave irradiation at 140° C. for 30 min. Silica gel was added and the solvents were removed under reduced pressure. The mixture was purified by HPLC, using NH4OH buffers (Waters semi-prep LCMS) to give the title compound (27.4 mg, 42%) as a white solid.

出典