Trifluoroacetic acid → Methyl (3-bromo-4-nitrophenyl)acetate

HRID 494393ノート

反応式

HRID 494393 の反応式
[CH3:1][O:2][C:3](=[O:22])[CH:4]([C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([Br:21])[CH:13]=1)C(OC(C)(C)C)=O.FC(F)(F)C(O)=O.C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3](=[O:22])[CH2:4][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([Br:21])[CH:13]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 576832692-(3-Bromo-4-nitrophenyl)malonic acid tert-butyl ester methyl ester

生成物 1

HCID 23512304Methyl (3-bromo-4-nitrophenyl)acetate収率 94.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

The 2-(3-bromo-4-nitrophenyl)malonic acid tert-butyl ester methyl ester (1.18 g) obtained in Example 4 a) was dissolved in chloroform (10 mL), trifluoroacetic acid (10 g) was added thereto under ice-cooling, and the mixture was stirred at room temperature for 5 hours. The reaction mixture was poured gradually into ice and saturated aqueous sodium bicarbonate, and extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over sodium sulfate and concentrated to give the title compound (0.820 g) as a pale yellow oil.

後処理

  1. temperatureunder ice-cooling
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water and saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-add141723c084d18b251c5a51095c2a1
出典データセット
uspto-grants-2009_05
特許番号
US07538140B2

反応ノート

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