Tetrahydrofuran → 6-Chloro-3-nitropyridine-2-carbonitrile
反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([Cl:11])[N:3]=1.C1COCC1.[C-]#[Si+].[C:19]([Cu])#[N:20]>O.CN1C(=O)CCC1>[Cl:11][C:4]1[N:3]=[C:2]([C:19]#[N:20])[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=1参加物
7
反応条件
- 温度
- 180 °C
実験手順
2,6-dichloro-3-nitro-pyridine (2.5 g, 12.9 mmol) is taken up in a solvent mixture of THF and NMP (5:1, 13 mL), combined with two spatula tips of silicon carbide and CuCN (2.3 g, 26.0 mmol) and heated to 180° C. in the microwave reactor for 45 min. Then the solid obtained is suspended in H2O, extracted with ethyl acetate, washed with NaCl-sln., the organic phase is dried on MgSO4, the solvent is eliminated in vacuo and 6-chloro-3-nitro-pyridine-2-carbonitrile (HPLC-MS: tRet.=1.01 min, MS(M+H)+=182, method LCMSBAS1) is obtained.
後処理
- customThen the solid obtained
- extractionextracted with ethyl acetate
- washwashed with NaCl-sln
- custom, the organic phase is dried on MgSO4
出典と根拠
- ORDレコード
- ord-2fdef5b7fcb34352928a4433b75f0f57
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637549B2
反応ノート
読み込み中…