反应详情

温度

25 °C

2-(Methylamino)ethanol (9.5 g, 7 equivalents) is added to a stirred mixture of 4-[(8-bromooctanoyl)amino]benzamide (5.76 g, 16.9 mmol, e.g. which can be as prepared in Intermediate 53 (first or alternative preparation thereof)) and dimethyl sulfoxide (30 mL). The mixture is stirred at 25° C. until the reaction is substantially complete and is then diluted with acetonitrile (115 mL). After stirring for 1 hour the mixture is filtered, washed with ethyl acetate (15 mL) and tert-butyl methyl ether (TBME, 15 mL) before being dried in vacuo to yield the title compound, generally as a solid.

1. customalternative preparation
2. stirringAfter stirring for 1 hour the mixture
3. filtrationis filtered
4. washwashed with ethyl acetate (15 mL) and tert-butyl methyl ether (TBME, 15 mL)
5. custombefore being dried in vacuo