(Bis(2-methoxyethyl)amino)sulfur trifluoride → HCID 58387952、化合物
反応式
COCCN(S(F)(F)[F:11])CCOC.[CH3:14][O:15][C:16](=[O:27])[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24]O)=[N:19][C:18]=1[NH2:26]>ClCCl>[CH3:14][O:15][C:16](=[O:27])[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][F:11])=[N:19][C:18]=1[NH2:26]参加物
4
実験手順
A solution of (bis(2-methoxyethyl)amino)sulfur trifluoride (2.39 g, 10.8 mmol) in dichloromethane (30 mL) was cooled with a dry ice-methanol bath, and 2-amino-6-(2-hydroxyethyl)-nicotinic acid methyl ester (50 mg, 0.255 mmol) was added thereto dropwise. After dropwise addition the cold bath was immediately removed, and the solution was gradually allowed to room temperature. Water and ethyl acetate were added to the reaction solution, which was then partitioned. The organic layer was separated, the solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography, and the title compound (4 mg, 0.020 mmol, 7.9%) was obtained as a white solid.