Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → (R)-2-(6-chloro-5-cyano-3-fluoropyridin-2-ylamino)butanamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2,6-Dichloro-5-fluoro-3-pyridinecarbonitrile | HCID 2733849 | — |
| 반응물 | (2R)-2-aminobutanamide hydrochloride | HCID 16218339 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | (R)-2-(6-chloro-5-cyano-3-fluoropyridin-2-ylamino)butanamide | HCID 86666160 | 98.2% |
반응 단계
To the mixture of (R)-(−)-2-aminobutanamide hydrochloride (1.00 g, 7.2 mmol) and 2,6-dichloro-5-fluoro-3-pyridinecarbonitrile (0.92 g, 4.8 mmol) in 40 mL NMP added DIEA (2.5 mL, 14.4 mmol). The mixture was then sent to 100° C. for stirring for 1 h. The mixture was cooled to RT, and to it was poured 300 mL EtOAc. The mixture was washed with brine four times. The organic phase was dried, concentrated and purified using silica flash column (70% EtOAc-30% DCM) to isolate (R)-2-(6-chloro-5-cyano-3-fluoropyridin-2-ylamino)butanamide (1.21 g, 98% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09359375B2 |
| 출처 데이터셋 | uspto-grants-2016_06 |
| ORD ID | ord-3e3999361bb6441db89323c44ede302c |
| 출처 메모 | uspto-grants-2016_06 |