Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Lithium Hydroxide → 1-((Tert-butoxy)carbonyl)-4,4-difluoropiperidine-2-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | 1-Tert-butyl 2-methyl 4,4-difluoropiperidine-1,2-dicarboxylate | HCID 49761285 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-((Tert-butoxy)carbonyl)-4,4-difluoropiperidine-2-carboxylic acid | HCID 10106900 | — |
반응 단계
To a solution of 1-tert-butyl 2-methyl 4,4-difluoropiperidine-1,2-dicarboxylate, 13e, (4.6 g, 16.5 mmol) in THF (18 mL), methanol (18 mL) and H2O (9 mL) was added lithium hydroxide (3.45 g, 82.22 mmol). The reaction mixture was stirred at room temperature for 1 hour. All volatiles were removed under reduced pressure. The residue was diluted with a slight amount of water and ether. The layers were separated and the organic phase was discarded. The aqueous phase was acidified to pH 3 with the addition of aqueous saturated KHSO4 solution. The product was extracted with EtOAc. The organic phase was washed with water, dried over MgSO4, filtered and evaporated to dryness. The resulting product was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08829007B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-20b677953a494242ab1dc23acc184e4c |
| 출처 메모 | uspto-grants-2014_09 |