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Sodium Acetate → ethyl 1-[2-oxo-2-({2-oxo-2-[3-(trifluoromethyl)phenyl]ethyl}amino)ethyl]-1H-pyrazole-4-carboxylate

HRID 1257427
ノート
印刷プレビュー

反応式

HRID 1257427 の反応式
Cl[C:2](=[O:14])[CH2:3][N:4]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[N:5]1.[NH2:15][CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)=[O:18].C([O-])(=O)C.[Na+]>ClCCl.O>[O:14]=[C:2]([NH:15][CH2:16][C:17](=[O:18])[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:27])([F:28])[F:26])[CH:20]=1)[CH2:3][N:4]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[N:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 517045Sodium AcetateHCID 133658842-Amino-1-[3-(trifluoromethyl)phenyl]ethanoneHCID 58127969HCID 58127969、化合物

生成物 1

HCID 58127653ethyl 1-[2-oxo-2-({2-oxo-2-[3-(trifluoromethyl)phenyl]ethyl}amino)ethyl]-1H-pyrazole-4-carboxylate収率 16.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

The compound (3.2 g) obtained in Example 115c and 2-amino-1-[3-(trifluoromethyl)phenyl]ethanone (2.88 g) were dissolved in dichloromethane (120 mL) and water (40 ml), and an aqueous solution (40 mL) of sodium acetate (2.46 g) was added dropwise under cooling in an ice bath. The reaction mixture was stirred at room temperature overnight, and the organic layer was separated, dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.92 g) as a colorless solid.

後処理

  1. temperatureunder cooling in an ice bath
  2. customthe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)

出典と根拠

ORDレコード
ord-486c954e01534f8f976f98530fd0fe90
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

反応ノート

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