Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Peroxide → 4-((1R,2S)-2-aminocyclohexylamino)-2-(1-methyl-1H-pyrazol-4-ylamino)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | tert-butyl (1S,2R)-2-(4-cyano-3-(1-methyl-1H-pyrazol-4-ylamino)phenylamino)cyclohexylcarbamate | HCID 68077202 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-((1R,2S)-2-aminocyclohexylamino)-2-(1-methyl-1H-pyrazol-4-ylamino)benzamide | HCID 57334335 | 78.7% |
반응 단계
To a solution of tert-butyl (1S,2R)-2-(4-cyano-3-(1-methyl-1H-pyrazol-4-ylamino)phenylamino)cyclohexylcarbamate (50 mg, 0.12 mmol) in DMSO (1 mL), K2CO3 (100 mg, 0.724 mmol) and H2O2 (50% aq., 0.800 mL) were added. The mixture was stirred at 100 C for 10 min. Water and EtOAc were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was dissolved in TFA (1 mL). After 10 min of standing, TFA was removed in vacuo. The residue was purified by HPLC to give the titled compound (31 mg). MS 329.4 (M+H); UV 205.3, 258.4, 280.5, 327.9 nm
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846928B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-35395989d28942b78e83c11536ccb6c4 |
| 출처 메모 | uspto-grants-2014_09 |