HCID 178514518、化合物 → 2-(4-Bromo-2,6-dichlorophenyl)-7-fluoro-2H-pyrazolo[4,3-c]pyridine

HRID 626801ノート

反応式

HRID 626801 の反応式
[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

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was triturated with diethyl ether
  3. customthe solid obtained
  4. filtrationwas collected by filtration
  5. 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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