Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-methyl-4-(1H-pyrazol-1-yl)aniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pyrazole | HCID 1048 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | trans-N,N'-dimethyl-1,2-cyclohexanediamine | HCID 2733821 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 2-methyl-4-(1H-pyrazol-1-yl)aniline | HCID 14450261 | 70.3% |
반응 단계
A solution of intermediate 82 (200 mg, 0.7 mmol), 1H-pyrazole (95 mg, 2 eq), CuI (133 mg, 1 eq), K2CO3 (290 mg, 2.1 eq) and (1R,2R)-diaminomethylcyclohexane (100 mg, 1 eq) in anh. NMP (1 mL), under N2, was heated at 150° C. for 6 hr. It was cooled down to r.t. and poured into water. EtOAc was added and the phases were separated. The aqueous layer was further extracted with EtOAc (2×10 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated. The residue was purified by flash-chromatography (silica gel, cHex/EtOAc 8:2) to give the title compound as a white solid (85.6 mg, 70%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07427630B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-2f001b2f271244129c6d25a97321b00c |
| 출처 메모 | uspto-grants-2008_09 |