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Dimethylformamide → HCID 66576211、化合物

HRID 1409355
ノート
印刷プレビュー

反応式

HRID 1409355 の反応式
[N:1]1[C:6]([C:7]([OH:9])=O)=[CH:5][CH:4]=[C:3]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:2]=1.[NH2:16][C@@H:17]([CH3:34])[CH2:18][N:19]1[CH:23]=[CH:22][C:21]([C:24]2[CH:31]=[C:30]([F:32])[C:27]([C:28]#[N:29])=[C:26]([Cl:33])[CH:25]=2)=[N:20]1.CN(C=O)C>C(Cl)Cl>[Cl:33][C:26]1[CH:25]=[C:24]([C:21]2[CH:22]=[CH:23][N:19]([CH2:18][C@@H:17]([NH:16][C:7]([C:6]3[N:1]=[CH:2][C:3]([C:10]4[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=4)=[CH:4][CH:5]=3)=[O:9])[CH3:34])[N:20]=2)[CH:31]=[C:30]([F:32])[C:27]=1[C:28]#[N:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 46316070[3,3'-Bipyridine]-6-carboxylic acidHCID 67170587(S)-4-(1-(2-aminopropyl)-1H-pyrazol-3-yl)-2-chloro-6-fluorobenzonitrile

生成物 1

HCID 66576211HCID 66576211、化合物収率 22.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The title compound was prepared using the procedure described in Example 3(h) starting from 3,3′-bipyridine-6-carboxylic acid (0.861 mmol, 172 mg) and (S)-4-(1-(2-aminopropyl)-1H-pyrazol-3-yl)-2-chloro-6-fluorobenzonitrile (0.718 mmol, 200 mg) using DMF (2 ml) as the solvent. After the reaction had stopped, DCM was added and the reaction mixture was evaporated. The residue was purified by flash chromatography and trituration from methanol, respectively. 75 mg of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 1.18 (d, 3H), 4.35-4.59 (m, 3H), 7.02 (d, 1H), 7.55-7.62 (m, 1H), 7.87-7.93 (m, 2H), 7.98 (s, 1H), 8.06-8.10 (m, 1H), 8.19-8.25 (m, 1H), 8.35 (dd, 1H), 8.68 (dd, 1H), 8.99-9.05 (m, 2H), 9.13 (d, 1H).

後処理

  1. customThe title compound was prepared
  2. customthe reaction mixture was evaporated
  3. customThe residue was purified by flash chromatography and trituration from methanol

出典と根拠

ORDレコード
ord-43da0785fbbb4671862403b83cd6fbd7
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921378B2

反応ノート

読み込み中…

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