Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3,5-Dimethylaniline → tert-butyl (1S,2R)-2-(4-cyano-3-(3,5-dimethylphenylamino)phenylamino)cyclohexylcarbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3,5-Dimethylaniline | HCID 7949 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | tert-butyl (1S,2R)-2-(3-bromo-4-cyanophenylamino)cyclohexylcarbamate | HCID 69283621 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | tert-butyl (1S,2R)-2-(4-cyano-3-(3,5-dimethylphenylamino)phenylamino)cyclohexylcarbamate | HCID 69283629 | — |
반응 단계
A mixture of tert-butyl (1S,2R)-2-(3-bromo-4-cyanophenylamino)cyclohexylcarbamate (150 mg, 0.380 mmol), 3,5-dimethylaniline (95 uL, 0.761 mmol), BINAP (40 mg, 0.064 mmol), Pd(OAc)2 (25 mg, 0.11 mmol) and K2CO3 (150 mg, 1.08 mmol) in dioxane (4 mL) was degassed with Ar, then was stirred at 100 C for 4 h. EtOAc and water were added. The organic phase was separated, washed with 1N HCl, then with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo to give tert-butyl (1S,2R)-2-(4-cyano-3-(3,5-dimethylphenylamino)phenylamino)cyclohexylcarbamate as a crude residue.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846928B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-03d7974576cd4c959a67de3464264e0b |
| 출처 메모 | uspto-grants-2014_09 |