HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → (E)-methyl 4-(cyclobutylamino)but-2-enoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Cyclobutylamine | HCID 75645 | — |
| Reactant | 2-Butenoic acid, 4-bromo-, methyl ester | HCID 5369175 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (E)-methyl 4-(cyclobutylamino)but-2-enoate | HCID 86689033 | 33.5% |
Reaction Steps
To a solution of (E)-methyl 4-bromobut-2-enoate (5.37 g, 30 mmol) in THF (60 mL) was added potassium carbonate (8.34 g, 60 mmol), followed by cyclobutanamine (2.13 g, 30 mmol, in 30 mL THF) under N2 atmosphere. The resulting reaction mixture was stirred at RT overnight. Excess potassium carbonate was removed by filtration and the filtrate was diluted with EA and water. The organic layer was separated and the aqueous later was extracted with EA. The combined organic phase was dried over Na2SO4. Solvent was removed in vacuum and the crude mixture was purified by flash chromatography (0-5% DCM/MeOH) to provide (E)-methyl 4-(cyclobutylamino)but-2-enoate (19) (1.7 g, 33%) as an oil. LC-MS (ESI): m/z (M+1), 170.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273051B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-455f9360bcfc4aa1942a1395b3f4b990 |
| Source note | uspto-grants-2016_03 |