Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → (R)-2-(4-cyano-3-(3-methylisothiazol-5-ylamino)phenylamino)-3-cyclohexylpropanamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | 3-Methylisothiazol-5-ylamine hydrochloride | HCID 2723918 | — |
| 반응물 | HCID 67509667 | HCID 67509667 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (R)-2-(4-cyano-3-(3-methylisothiazol-5-ylamino)phenylamino)-3-cyclohexylpropanamide | HCID 67509014 | 99.1% |
반응 단계
A mixture of (R)-2-(3-bromo-4-cyanophenylamino)-3-cyclohexylpropanamide (222 mg, 0.634 mmol), 5-amino-3-methylisothiazole hydrochloride (126 mg, 0.840 mmol), BINAP (60 mg, 0.096 mmol), Pd(OAc)2 (45 mg, 0.200 mmol) and K2CO3 (360 mg, 2.60 mmol) in dioxane (4 mL) was degassed with Ar, then was stirred at 120 C for 18 h. Water and EtOAc were added. After being filtered, the organic phase was separated, washed with 1N HCl, then with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo to give (R)-2-(4-cyano-3-(3-methylisothiazol-5-ylamino)phenylamino)-3-cyclohexylpropanamide as a solid (241 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09359375B2 |
| 출처 데이터셋 | uspto-grants-2016_06 |
| ORD ID | ord-53e9a1bed58b444681c0bc95a30604fe |
| 출처 메모 | uspto-grants-2016_06 |