反应详情

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.

1. temperatureBoiling under reflux
2. concentrationthe mixture is concentrated in a rotary evaporator
3. customreacted with 150 ml 25% Nh4OH solution
4. extractionExtraction with dichloromethane
5. dry with materialthe combined extracts are dried over calcium carbonate
6. concentrationconcentrated in a rotary evaporator