関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 3-Fluorobenzylamine | HCID 66853 | — |
| 反応物 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Chloro-6-(3-fluorobenzylamino)isonicotinonitrile | HCID 83073097 | 99.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08415381B2 |
|---|
| 出典データセット | uspto-grants-2013_04 |
|---|
| ORD ID | ord-dd0363d8da1544b588d6c72e1f2f28a4 |
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| 出典メモ | uspto-grants-2013_04 |
|---|
