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Trifluoroacetic acid → Methyl 2-(3-(dimethylcarbamoyl)-4-nitrophenyl)acetate

HRID 494390
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HRID 494390 반응식
[CH3:1][O:2][C:3](=[O:26])[CH:4]([C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([C:21](=[O:25])[N:22]([CH3:24])[CH3:23])[CH:13]=1)C(OC(C)(C)C)=O.FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][C:3](=[O:26])[CH2:4][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([C:21](=[O:25])[N:22]([CH3:24])[CH3:23])[CH:13]=1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 687608552-(3-Dimethylcarbamoyl-4-nitrophenyl)malonic acid tert-butyl ester methyl ester

생성물 1

HCID 57683227Methyl 2-(3-(dimethylcarbamoyl)-4-nitrophenyl)acetate수율 80.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

The 2-(3-dimethylcarbamoyl-4-nitrophenyl)malonic acid tert-butyl ester methyl ester (1.22 g) obtained in Example 2b) was dissolved in dichloromethane (10 mL), and the solution was cooled to 0° C. After addition of trifluoroacetic acid (10 mL), the mixture was stirred at room temperature for 6 hours, and concentrated, followed by azeotropic distillation with toluene. The residue was purified by column chromatography on silica gel with ethyl acetate:hexane=3:1 to give the title compound (712 mg).

후처리

  1. concentrationconcentrated
  2. distillationfollowed by azeotropic distillation with toluene
  3. customThe residue was purified by column chromatography on silica gel with ethyl acetate

출처 및 근거

ORD 기록
ord-82bd61dfd8e344c5b49681ce50dda503
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538140B2

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