참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | 3-Fluorobenzylamine | HCID 66853 | — |
| 반응물 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Chloro-6-(3-fluorobenzylamino)isonicotinonitrile | HCID 83073097 | 99.2% |
반응 단계
To a scintillation vial containing 2,6-dichloroisonicotinonitrile (500 mg, 2.89 mmol) was added NMP (6 ml) and (3-fluorophenyl)methanamine (868 mg, 6.94 mmol). The homogenous reaction mixture was capped and heated to 110° C. in a oil bath for 1 hr. The reaction mixture was diluted with EtOAc and washed with sat NaHCO3, H2O and sat NaCl. The organic layer was dried Na2SO4, filtered and concentrated. The crude residue was purified by column chromatography on silica gel (0-20% EtOAc/Hexane) to give 2-chloro-6-(3-fluorobenzylamino)isonicotinonitrile (750 mg, 95%). LCMS (m/z): 262.0 (MH+), retention time=1.03 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08415381B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_04 |
|---|
| ORD ID | ord-dd0363d8da1544b588d6c72e1f2f28a4 |
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| 출처 메모 | uspto-grants-2013_04 |
|---|
