Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroethane → 1-Ethyl-4-(3-cyano-4-fluorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroethane | HCID 6337 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-(3-Cyano-4-fluorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile | HCID 59763246 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Ethyl-4-(3-cyano-4-fluorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile | HCID 69042556 | — |
반응 단계
To a solution of 4-(3-cyano-4-fluorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile (1 eq), from Synthetic Example 1, in DMF was added either NaH or Cs2CO3 (1.2 eq) at 0° C. After 30 min, ethyl chloride was introduced. The reaction mixture was stirred at rt overnight, and quenched with brine. The reaction mixture was extracted with EtOAc, washed with brine, and dried. Concentration followed by flash chromatography gave 1-ethyl-4-(3-cyano-4-fluorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile. 1H-NMR (400 MHz, DMSO-D6): δ=7.86 (dd, 1H), 7.69 (m, 1H), 7.55 (t, 1H), 4.57 (s, 1H), 3.12 (q, 2H), 2.1 (s, 6H), 1.4 (t, 3H) ppm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08198456B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-69f6b9f24fd540fa94884e5aada17ec3 |
| 출처 메모 | uspto-grants-2012_06 |