Methanol → HCID 86746632, compound

Participants

Reaction Steps

430 ml methanol are cooled to -10° C. in an ice/sodium chloride mixture and reacted with 21.3 ml thionyl chloride (exothermic reaction). 44.5 g (0.23 mol) α-methyl-homo-phenylalanine are added dropwise at room temperature. Boiling under reflux occurs for 8.5 hours, the mixture is concentrated in a rotary evaporator, taken up with H2O (350 ml) and reacted with 150 ml 25% NH4OH solution. Extraction with dichloromethane occurs 5× and the combined extracts are dried over calcium carbonate and concentrated in a rotary evaporator. Yellowish oil.

Provenance & Evidence