反应详情

温度

35 °C

Trifluoroacetic acid (17.4 mL, 234 mmol) was added carefully to a stirred mixture of Boc aldehyde 1-4 (20 g, 78.1 mmol) and dichloromethane (60 mL) keeping the temperature below 25° C. The solution was warmed to 35° C., aged overnight (vigorous off-gassing) and then cooled to room temperature. 25 mL of MTBE was added and the resulting white slurry was aged for one hour, filtered, and the filter cake rinsed with MTBE (10 mL×2). Solid 1-5c TFA salt was dried under vacuum.

1. customthe temperature below 25° C
2. temperaturecooled to room temperature
3. filtrationfiltered
4. washthe filter cake rinsed with MTBE (10 mL×2)
5. dry with materialSolid 1-5c TFA salt was dried under vacuum