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

HRID 132028

反応式

HRID 132028 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.[F:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([C:22]2[C:26]([NH2:27])=[CH:25][NH:24][N:23]=2)=[O:21])=[CH:15][CH:14]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[F:12][C:13]1[CH:14]=[CH:15][C:16]([NH:19][C:20]([C:22]2[C:26]([NH:27][C:5](=[O:7])[C:4]3[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=3[O:2][CH3:1])=[CH:25][NH:24][N:23]=2)=[O:21])=[CH:17][CH:18]=1

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 113702-Methoxybenzoic acidHCID 757711-HydroxybenzotriazoleHCID 178508056HCID 178508056、化合物

生成物 1

HCID 1784895554-(2-Methoxy-benzoylamino)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide収率 15%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-Methoxy-benzoic acid (38 mg, 0.25 mmol) was added to a solution of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (50 mg, 0.23 mmol), EDC (53 mg, 0.27 mmol), and HOBt (37 mg, 0.27 mmol) in DMF (5 ml). The reaction mixture was stirred at room temperature for 24 hours. The solvent was removed under reduced pressure. The residue was purified by preparative LC/MS and, after evaporation of product-containing fractions, yielded the product as a pinkish solid (12 mg, 15%). (LC/MS: Rt 4.00, [M+H]+354.67).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customThe residue was purified by preparative LC/MS
  3. customafter evaporation of product-containing fractions

出典と根拠

ORDレコード
ord-e1b19bd26763454f9e88b8793fd33fcf
出典データセット
uspto-grants-2008_06
特許番号
US07385059B2

関連ノート

読み込み中…