Oxalyl chloride → 2-Cyano-4-(trifluoromethyl)-5-pyrimidinecarbonyl chloride
반응식
[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]참가 물질
5
실험 절차
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).
후처리
- concentrationThe reaction was concentrated
- distillationdistilled (b.p. 100° C., 1.5 mm/Hg)
출처 및 근거
- ORD 기록
- ord-dd830d0144254084ac1e1e3106c68e28
- 출처 데이터셋
- uspto-grants-1998_09
- 특허 번호
- US05811428
반응 노트
불러오는 중…