Dimethylamine → [2-(4-Bromopyrazol-1-yl)ethyl]dimethylamine

温度

60 °C

4-bromopyrazole (100 mg, 0.680 mmol, available from Aldrich), cesium carbonate (333 mg, 1.021 mmol) and 1-bromo-2-chloroethane (0.085 mL, 1.021 mmol, available from Aldrich) were suspended in N,N-Dimethylformamide (DMF) (2 mL) and heated to 60° C. under microwave conditions in a Biotage Initiator for 1 hour. 2M dimethylamine in THF (1.701 mL, 3.40 mmol) added and the mixture allowed to stand over the weekend. The mixture was heated to 60° C. under microwave conditions in a Biotage Initiator for 1 hour, then to 100° C. under microwave conditions in a Biotage Initiator for 2 hours. The mixture was filtered, evaporated to 13 mbar, loaded on to a 5 g SCX cartridge and eluted with MeOH (25 ml) followed by 2M methanolic ammonia (25 ml). The basic fraction was evaporated to a colourless oil (99 mg). LCMS (Method C): Rt=0.43, MH+=218

1. temperatureThe mixture was heated to 60° C. under microwave conditions in a Biotage Initiator for 1 hour
2. filtrationThe mixture was filtered
3. customevaporated to 13 mbar
4. washeluted with MeOH (25 ml)
5. customThe basic fraction was evaporated to a colourless oil (99 mg)

ORDレコード

ord-360eede0cf3640b6bd1a848cd1891ae6

出典データセット

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08697725B2