HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl 3-allylamino-2-benzyloxycarbonylamino-2-methylpropionate → Methyl 3-amino-2-benzyloxycarbonylamino-2-methylpropionate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl 3-allylamino-2-benzyloxycarbonylamino-2-methylpropionate | HCID 68691822 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 3-amino-2-benzyloxycarbonylamino-2-methylpropionate | HCID 68692239 | 83.9% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652007B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-20e83a8ebfc3406f8c36920650cb261d |
| Source note | uspto-grants-2010_01 |