Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Hydroxide → 4-(4-Oxopiperidin-1-yl)benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 4-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-benzoic acid | HCID 15948425 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 생성물 | 4-(4-Oxopiperidin-1-yl)benzoic acid | HCID 22064022 | 88.3% |
반응 단계
4-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-benzoic acid(which was obtained in Example 150) (12.5 g, 47.5 mmol) was treated with concentrated hydrochloric acid (500 mL) at room temperature. After 15 hours ˜28% ammonium hydroxide was added dropwise and the precipitate was collected by filtration, and dried over phosphorus pentoxide to give the title compound as a white solid (9.2 g, 88%); 1H NMR (300 MHz, CDCl3) δ 2.46 (t, J=6.1 Hz, 4H), 3.74 (t, J=6.1 Hz, 4H), 7.02 (d, J=9.0 Hz, 2H), 7.80 (d, J=9.0 Hz, 2H); MS (ES) m/z: 219.8 (MH+); HRMS Calcd. for C12H14NO3 (MH+): 220.0974. Found: 220.0947.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06525202B2 |
| 출처 데이터셋 | uspto-grants-2003_02 |
| ORD ID | ord-4c61c1d8e6c048f0950e4166de7c5707 |
| 출처 메모 | uspto-grants-2003_02 |