反応 #166417

反応方程式

triethylamine

compound 405

4-methyl-1-oxa-4,9-diazaspiro[5.5]undecane

3,6-dichloropyridazine

→

compound 406

収率 45.0%

9-(6-chloro-3-pyridazinyl)-4-methyl-1-oxa-4,9-diazaspiro[5.5]undecane

収率 45.0%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度at reflux for 38 hours
2. 2
   濃縮The reaction mixture was then concentrated
3. 3
   その他the residue was purified by reverse phase HPLC (acetonitrile/H2O containing 0.1% TFA each, 25 min from 10 to 40%)

実験手順

To a solution of compound 405 (406.0 mg, 2.39 mmol) in tetrahydrofuran (17 mL) was added 3,6-dichloropyridazine (361.7 mg, 2.43 mmol), followed by triethylamine (0.680 mL, 4.89 mmol). The resulting solution was stirred at reflux for 38 hours. The reaction mixture was then concentrated and the residue was purified by reverse phase HPLC (acetonitrile/H2O containing 0.1% TFA each, 25 min from 10 to 40%) to give compound 406 as a sticky yellow solid (303 mg, 45%). LCMS-ESI (POS), M/Z, M+1: Found 283.1, Calculated 283.1.

出典