Oxalyl chloride → 2-Cyano-4-(trifluoromethyl)-5-pyrimidinecarbonyl chloride
反応式
[C:1]([C:3]1[N:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[C:6]([C:13]([OH:15])=O)=[CH:5][N:4]=1)#[N:2].C(Cl)(=O)C([Cl:19])=O>CN(C=O)C.ClCl>[C:1]([C:3]1[N:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[C:6]([C:13]([Cl:19])=[O:15])=[CH:5][N:4]=1)#[N:2]参加物
5
実験手順
A solution of 2-cyano-4-trifluoromethylpyrimidine-5-carboxylic acid (2.0 g, 9.2 mmol), oxalyl chloride (1.4 g, 11 mmol) and DMF (4 drops) in CH2 Cl2 (46 mL) was stirred at room temperature under N2 for 0.75 h. The reaction was concentrated and distilled (b.p. 100° C., 1.5 mm/Hg) to give the title compound (1.8 g, 82% yield); 1HNMR (CDCl3) δ 9.49 (s, 1H).
後処理
- concentrationThe reaction was concentrated
- distillationdistilled (b.p. 100° C., 1.5 mm/Hg)
出典と根拠
- ORDレコード
- ord-dd830d0144254084ac1e1e3106c68e28
- 出典データセット
- uspto-grants-1998_09
- 特許番号
- US05811428
反応ノート
読み込み中…