Methylamine → [(2,6-Dichloropyridin-3-yl)methyl](methyl)amine

In 50 ml of acetonitrile was dissolved 7.8 g (0.1 mole) of 40% aqueous methylamine and with stirring and ice-cooling, a solution of 3.9 g (0.02 mole) of 2,6-dichloro-3-pyridylmethyl chloride in 10 ml of acetonitrile was added dropwise over 5 minutes. After completion of the dropwise addition, the mixture was stirred at room temperature for 2 hours and, then, concentrated. The residue was extracted with ether (30 ml×3) and dried over MgSO4. Finally, the solvent was distilled off to give 3.2 g of the title compound as a pale yellow oil.

1. temperatureice-cooling
2. additionAfter completion of the dropwise addition
3. stirringthe mixture was stirred at room temperature for 2 hours
4. concentrationconcentrated
5. extractionThe residue was extracted with ether (30 ml×3)
6. dry with materialdried over MgSO4
7. distillationFinally, the solvent was distilled off

ORDレコード

ord-ab6497bd9ace42d8ae0d80948a8c2c49

出典データセット

uspto-grants-1993_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05214152