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Sodium hydride → Propanedioic acid, 2-(5-chloro-2,4-dinitrophenyl)-, 1-(1,1-dimethylethyl) 3-ethyl ester

HRID 1773532
ノート
印刷プレビュー

反応式

HRID 1773532 の反応式
[H-].[Na+].[C:3]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[Cl:16][C:17]1[CH:22]=[C:21](Cl)[C:20]([N+:24]([O-:26])=[O:25])=[CH:19][C:18]=1[N+:27]([O-:29])=[O:28]>CN1CCCC1=O>[CH2:8]([O:7][C:5](=[O:6])[CH:4]([C:21]1[CH:22]=[C:17]([Cl:16])[C:18]([N+:27]([O-:29])=[O:28])=[CH:19][C:20]=1[N+:24]([O-:26])=[O:25])[C:3]([O:11][C:12]([CH3:14])([CH3:13])[CH3:15])=[O:10])[CH3:9]
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 24758Sodium hydrideHCID 772861,3-Dichloro-4,6-dinitrobenzeneHCID 96345tert-Butyl ethyl malonate

生成物 1

HCID 86661368Propanedioic acid, 2-(5-chloro-2,4-dinitrophenyl)-, 1-(1,1-dimethylethyl) 3-ethyl ester収率 64.6%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

Sodium hydride (60% suspension in mineral oil, 1.60 mmol) was added to a mixture of tert-butyl ethyl malonate (300 mg) in 1-methyl-2-pyrrolidinone (3 mL) and was followed by 1,5-dichloro-2,4-dinitrobenzene (0.45 g). The reaction mixture was stirred for 15 minutes and was then quenched by addition of a diluted aqueous solution of hydrochloric acid. The resulting mixture was extracted with ethyl acetate; the combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography (EtOAc/hexane, 5/95 to 15/85) to give 0.4 g of 2-(5-chloro-2,4-dinitro-phenyl)-malonic acid tert-butyl ester ethyl ester.

後処理

  1. customwas then quenched by addition of a diluted aqueous solution of hydrochloric acid
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. washthe combined organic extracts were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe residue was purified by flash chromatography (EtOAc/hexane, 5/95 to 15/85)

出典と根拠

ORDレコード
ord-66d4b6856f20489aba57d74b05357619
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09255110B2

反応ノート

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