HCID 178514518、化合物 → 2-(4-Bromo-2,6-dichlorophenyl)-7-fluoro-2H-pyrazolo[4,3-c]pyridine
反応式
[N:1]([C:4]1[C:9]([F:10])=[CH:8][N:7]=[CH:6][C:5]=1/[CH:11]=[N:12]/[C:13]1[C:18]([Cl:19])=[CH:17][C:16]([Br:20])=[CH:15][C:14]=1[Cl:21])=[N+]=[N-]>C1(C)C=CC=CC=1>[Br:20][C:16]1[CH:17]=[C:18]([Cl:19])[C:13]([N:12]2[CH:11]=[C:5]3[CH:6]=[N:7][CH:8]=[C:9]([F:10])[C:4]3=[N:1]2)=[C:14]([Cl:21])[CH:15]=1参加物
3
実験手順
A solution of [1-(4-azido-5-fluoropyridin-3-yl)meth-(E)-ylidene]-(4-bromo-2,6-dichlorophenyl)amine (˜60 mmol) in toluene (200 mL) was heated at 105° C. for 2 hours. The resultant mixture was cooled to room temperature and concentrated under reduced pressure. The residue was triturated with diethyl ether and the solid obtained was collected by filtration and dried to afford the title compound (14.5 g, 67% yield over two steps). 1H NMR (400 MHz, DMSO-d6): δ 9.25 (d, J=2.7 Hz, 1H), 9.20 (d, J=2.6 Hz, 1H), 8.28 (dd, J=3.8, 0.5 Hz, 1H), 8.19 (s, 2H).
後処理
- concentrationconcentrated under reduced pressure
- customThe residue was triturated with diethyl ether
- customthe solid obtained
- filtrationwas collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-9997b47a75ec42a0bffd133255ac0633
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309240B2
反応ノート
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