Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → (E)-methyl 4-(cyclobutylamino)but-2-enoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Cyclobutylamine | HCID 75645 | — |
| 반응물 | 2-Butenoic acid, 4-bromo-, methyl ester | HCID 5369175 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (E)-methyl 4-(cyclobutylamino)but-2-enoate | HCID 86689033 | 33.5% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08377946B1 |
| 출처 데이터셋 | uspto-grants-2013_02 |
| ORD ID | ord-86e2bcdc26d742df83851a1f583167be |
| 출처 메모 | uspto-grants-2013_02 |