反应详情

In a three-necked flask, mix N-[2-(3,4-dimethoxyphenyl)ethyl]-2,2,2-trifluoroacetamide (35 g, 126 mmoles) and 37% aqueous formaldehyde (776 mL, 1.014 mole) in 120 mL of dichloromethane at 0° C. To the resulting two-phase mixture slowly add, at 0° C., 345 mL of 37% aqueous hydrochloric acid solution and heat at 40° C. After being in contact for 3 hours, hydrolyse the mixture using 250 mL of water and wash the aqueous phase with dichloromethane (2×100 mL). Combine the organic phases, dry them over MgSO4 and carry out drying in vacuo to obtain a beige meringue (38.2 g). The product obtained is recrystallised from toluene to obtain 31.5 g of a white powder corresponding to the title compound.

1. additionTo the resulting two-phase mixture slowly add, at 0° C.
2. washwash the aqueous phase with dichloromethane (2×100 mL)
3. dry with materialCombine the organic phases, dry them over MgSO4
4. customcarry out drying in vacuo
5. customto obtain a beige meringue (38.2 g)
6. customThe product obtained
7. customis recrystallised from toluene