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

HRID 342616
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HRID 342616 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]
참가 물질실험 절차후처리출처 및 근거반응 노트

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 mixture of 45.3 g of diethyl (2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)malonate, 30 mg of p-toluenesulfonic acid, and 120 ml of water was heated under reflux for 50 minutes. After cooling, the reaction mixture was extracted with diethyl ether, and the extract was washed with brine, and then dried and concentrated to give 34.2 g of brown oil.

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후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 50 minutes
  3. temperatureAfter cooling
  4. extractionthe reaction mixture was extracted with diethyl ether
  5. washthe extract was washed with brine
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8863449dc13f40c1b1d081be03754d1b
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859026

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