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p-Toluenesulfonic acid → Ethyl (2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acetate

HRID 1078265
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HRID 1078265 반응식
[F:1][C:2]1[C:20]([CH3:21])=[C:19]([F:22])[C:18]([F:23])=[C:17]([N+:24]([O-:26])=[O:25])[C:3]=1[C:4]([CH:6](C(OCC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[F:1][C:2]1[C:20]([CH3:21])=[C:19]([F:22])[C:18]([F:23])=[C:17]([N+:24]([O-:26])=[O:25])[C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]
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참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 11793970Diethyl (2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)malonate

생성물 1

HCID 10590663Ethyl (2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acetate수율 93.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A suspension of 45.3 g of diethyl (2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)malonate and 30 mg of p-toluenesulfonic acid in 120 ml of water was heated at reflux for 50 minutes. After cooling, the reaction mixture was extracted with diethyl ether. The combined organic extracts were washed with brine, dried and evaporated to give 34.2 g of the desired compound as brown oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 50 minutes
  3. temperatureAfter cooling
  4. extractionthe reaction mixture was extracted with diethyl ether
  5. washThe combined organic extracts were washed with brine
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-5eb8e74a998c49aa973b54735318eb10
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05547962

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