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Semicarbazide hydrochloride → [(E)-1-[3-[difluoro(quinolin-6-yl)methyl]-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]ethylideneamino]urea

HRID 456098
ノート
印刷プレビュー

反応式

HRID 456098 の反応式
[F:1][C:2]([F:25])([C:15]1[CH:16]=[C:17]2[C:22](=[CH:23][CH:24]=1)[N:21]=[CH:20][CH:19]=[CH:18]2)[C:3]1[N:7]2[N:8]=[C:9]([C:12](=O)[CH3:13])[CH:10]=[CH:11][C:6]2=[N:5][N:4]=1.Cl.[NH:27]([C:29]([NH2:31])=[O:30])[NH2:28]>CO>[F:1][C:2]([F:25])([C:15]1[CH:16]=[C:17]2[C:22](=[CH:23][CH:24]=1)[N:21]=[CH:20][CH:19]=[CH:18]2)[C:3]1[N:7]2[N:8]=[C:9](/[C:12](=[N:28]/[NH:27][C:29]([NH2:31])=[O:30])/[CH3:13])[CH:10]=[CH:11][C:6]2=[N:5][N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11236Semicarbazide hydrochlorideHCID 581904681-(3-(Difluoro(quinolin-6-yl)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone

生成物 1

HCID 71699895[(E)-1-[3-[difluoro(quinolin-6-yl)methyl]-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]ethylideneamino]urea収率 77%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1-(3-(difluoro(quinolin-6-yl)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (100 mg, 0.295 mmol) and hydrazinecarboxamide hydrochloride (44.3 mg, 0.589 mmol) in MeOH was stirred at room temperature for overnight. Solvent was evaporated and the residue was dissolved in a small amount of MeOH. Solid was filtered and dried to give the title compound as a white solid (90 mg, 75%). 1H-NMR (400 MHz, DMSO-d6) δ ppm 9.90 (s, 1H), 9.06 (d, 1H), 8.62 (d, 1H), 8.49 (m, 2H), 8.34 (d, 1H), 8.20 (d, 1H), 8.03 (d, 1H), 7.70 (m, 1H), 6.82 (broad, 2H), 2.07 (s, 3H). LCMS (method B): [MH]+=397.1, tR=2.08 min.

後処理

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in a small amount of MeOH
  3. filtrationSolid was filtered
  4. customdried

出典と根拠

ORDレコード
ord-9840ba86a49847e2a13f26c4afb4d803
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08497368B2

反応ノート

読み込み中…

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