1,2-Dichloroethane → 4-(2-fluoro-3-methoxy-benzoylamino)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

HRID 132031

反応式

HRID 132031 の反応式
[F:1][C:2]1[C:10]([O:11][CH3:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[F:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([C:23]2[C:27]([NH2:28])=[CH:26][NH:25][N:24]=2)=[O:22])=[CH:16][CH:15]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CS(C)=O.O>[F:13][C:14]1[CH:15]=[CH:16][C:17]([NH:20][C:21]([C:23]2[C:27]([NH:28][C:4](=[O:6])[C:3]3[CH:7]=[CH:8][CH:9]=[C:10]([O:11][CH3:12])[C:2]=3[F:1])=[CH:26][NH:25][N:24]=2)=[O:22])=[CH:18][CH:19]=1

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 33906792-Fluoro-3-methoxybenzoic acidHCID 178508056HCID 178508056、化合物

生成物 1

HCID 1784904924-(2-fluoro-3-methoxy-benzoylamino)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide収率 63%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

2-Fluoro-3-methoxybenzoic acid (0.047 g, 0.28 mmol), 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (Example 2B) (0.055 g, 0.25 mmol), EDC (0.58 g, 0.30 mmol) and HOBt (0.041 g, 0.30 mmol) were stirred at room temperature in DMSO (1.25 ml) for 5 hours. The reaction mixture was poured into water (30 ml) and the resultant solid was collected by filtration and dried in a vacuum oven to give the title compound as a grey solid (0.058 g, 63%). (LC/MS: Rt 3.99, [MH]+372.98).

後処理

  1. filtrationthe resultant solid was collected by filtration
  2. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-af9d758cc364422fa6f2013acb95b677
出典データセット
uspto-grants-2008_06
特許番号
US07385059B2

関連ノート

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