反应详情

A solution of 0.22 g (1.42 mmol) of N,N-dimethylbarbituric acid, 0.02 g (0.017 mmol) of Pd(PPh3)4, 1.5 ml of DCM and 0.145 g (0.47 mmol) of methyl 3-allylamino-2-benzyloxycarbonylamino-2-methylpropionate is heated at 35° C. for 2 h. The reaction solution is subsequently concentrated in vacuo, and then 20 ml of diethyl ether are added, and the solution is washed 3 times with 20 ml of saturated Na2CO3 each time. A pH of 2 is adjusted by dropwise addition of 4N HCl. The aqueous phase is separated off and extracted with 2 ml of EtOAc, and the solvent is removed in vacuo. 0.105 g of the desired product are obtained. MW (calculated, monoisotopic)=266, measured value: (M+H)+ 267.

1. concentrationThe reaction solution is subsequently concentrated in vacuo
2. addition20 ml of diethyl ether are added
3. washthe solution is washed 3 times with 20 ml of saturated Na2CO3 each time
4. additionA pH of 2 is adjusted by dropwise addition of 4N HCl
5. customThe aqueous phase is separated off
6. extractionextracted with 2 ml of EtOAc
7. customthe solvent is removed in vacuo