Ammonium Chloride → HCID 54596448, compound

Participants

Reaction Steps

4-Bromo-2-(3,5-dichlorophenyl)-5-methoxypyridazin-3-one (2.5 g, 0.0071 moles) was dissolved in THF (250 ml) and cooled to −50° under nitrogen. 1.6M n-Butyl lithium (6.7 ml, 0.011 moles) was added dropwise with stirring. Allowed to warm to −20° over 1 hour. Added 1 equivalent of 1.6M n-Butyl lithium (4.4 ml, 0.0071 moles) dropwise. Stirred at −20° for 30 minutes. Poured into ammonium chloride solution and stirred for 15 minutes. Extracted with EtOAc (×2) and washed with water. Dried over anhydrous magnesium sulphate, filtered and evaporated to give a brown solid. (3.0 g) Purified using MPLC (silica, eluted with dichloromethane: EtOAc 9:1) to give a yellow solid. (0.25 g, 13%) Not pure used directly in the next reaction.

Provenance & Evidence