Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → {(2S,4R)-1-[(1S,4R)-5-(Benzyloxy)-4-methyl-1-(3,3,3-trifluoropropyl)pent-2-yn-1-yl]-2-[4-(trifluoromethyl)phenyl]piperidin-4-yl}acetic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methyl {(2S,4R)-1-[(1S)-5-(benzyloxy)-4-methyl-1-(3,3,3-trifluoropropyl)pent-2-yn-1-yl]-2-[4-(trifluoromethyl)phenyl]piperidin-4-yl}acetate | HCID 59201240 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | {(2S,4R)-1-[(1S,4R)-5-(Benzyloxy)-4-methyl-1-(3,3,3-trifluoropropyl)pent-2-yn-1-yl]-2-[4-(trifluoromethyl)phenyl]piperidin-4-yl}acetic acid | HCID 86639340 | 97.4% |
반응 단계
A solution of lithium hydroxide (19.7 mg, 0.822 mmol) in water (1 ml) was added to a stirred solution of the ester (Step 3, 96 mg, 0.164 mmol) in THF (2 ml) at RT. The mixture was stirred at RT o/n. 2N HCl (1 ml) was added The pH of the aqueous layer was adjusted to 7 with NaHCO3 (aq). The aqueous layer was extracted with DCM (×3). The combined extracts were dried (Na2SO4), filtered and evaporated. The residue was purified by chromatography (silica, 2-5% MeOH/DCM) to give the acid (91 mg) as a colourless oil. M/Z 570 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08389547B2 |
| 출처 데이터셋 | uspto-grants-2013_03 |
| ORD ID | ord-c3d065db92cc477e96bcba140c4e7388 |
| 출처 메모 | uspto-grants-2013_03 |