Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3-dimethyl-4-nitro-1H-pyrazole-5-carboxamide → 4-amino-1,3-dimethyl-1H-pyrazole-5-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3-dimethyl-4-nitro-1H-pyrazole-5-carboxamide | HCID 1229764 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-amino-1,3-dimethyl-1H-pyrazole-5-carboxamide | HCID 13822925 | 97.8% |
반응 단계
To a solution of 1,3-dimethyl-4-nitro-1H-pyrazole-5-carboxamide (730 mg, 3.96 mmol) in anhydrous ethanol (100 mL) and ethyl acetate (100 mL) was added 10 wt % Pd on carbon (100.0 mg). The reaction mixture was evacuated with vacuum and purged with H2 (3×), then stirred under H2 at 50 psi for 5 hours. The reaction mixture was then filtered through a pad of Celite®. The filtrate was concentrated in vacuo and the crude was purified by column chromotagraphy (Si-PPC, gradient 0 to 30% methanol in dichloromethane) to get the desired product (597.0 mg, 97.7%) as a solid. 1H NMR (DMSO-d6, 400 MHz) δ ppm 7.26 (br s, 2H), 4.03 (br s, 2H), 3.84 (s, 3H), 2.02 (s, 3H); LC-MS m/z (method A)=155.2 [M+H]+, RT=0.35 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08828990B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-81c88674567548589f2b42bc6eb3856d |
| 출처 메모 | uspto-grants-2014_09 |