Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Bromide → Clavulanic Acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 3-(2-Hydroxy-ethylidene)-7-oxo-4-oxa-1-aza-bicyclo[3.2.0]heptane-2-carboxylic acid benzyl ester(benzyl calvunlanate) | HCID 9904055 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Clavulanic Acid | HCID 5280980 | — |
반응 단계
Benzyl clavulanate (840 mgs) in ethanol (30 ml) and water (5 ml) was hydrogenated over 10% Pd/C (267 mgs) and sodium bicarbonate (244 mgs) for 25 minutes at room temperature and atmospheric pressure. The catalyst was filtered, washed with water and ethanol and the combined filtrates were evaporated in vacuo. The product crystallised from a water-acetone mixture as microneedles (565 mgs). Recrystallisation from water-acetone gave needles which, after drying over P2O5 in vacuo for 24 hours gave the following analysis: C 41.01, 40.86; H 3.77, 3.64; N 5.68, 5.51; i.r.(KBr disc) 1785, 1700, 1620 cm-1 ; Nmr (D2O) 3.06 (d,1,J=18.5 Hz), 3.57 (dd,1,J1 =18.5 Hz, J2 =2.5 Hz), 4.15 (d,2,J=8 Hz), 5.3 (HOD), 4.9(m), 5.71 (d,1,J=2.5 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04526783 |
| 출처 데이터셋 | uspto-grants-1985_07 |
| ORD ID | ord-245d07d2c781440a81b6e5d8c61452dc |
| 출처 메모 | uspto-grants-1985_07 |