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Ethanol, 1-ethoxy-2,2,2-trifluoro- → Trifluoroacetaldehyde {2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}hydrazone

HRID 253321
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HRID 253321 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([S:9][CH2:10][C:11]([F:14])([F:13])[F:12])=[CH:4][C:3]=1[NH:15][NH2:16].C(O[CH:20](O)[C:21]([F:24])([F:23])[F:22])C>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([S:9][CH2:10][C:11]([F:13])([F:14])[F:12])=[CH:4][C:3]=1[NH:15][N:16]=[CH:20][C:21]([F:24])([F:23])[F:22]
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참가 물질

5

반응물 2

HCID 9897Ethanol, 1-ethoxy-2,2,2-trifluoro-HCID 668419362-Chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenylhydrazine

생성물 1

HCID 86628937Trifluoroacetaldehyde {2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}hydrazone수율 67.8%

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 702Ethanol용매

실험 절차

A mixture of 4.1 g of 2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenylhydrazine, 2.3 g of trifluoroacetaldehyde ethyl hemiacetal, 0.1 g of p-toluenesulfonic acid monohydrate and 50 ml of ethanol was refluxed with heating for 6 hours. The obtained reaction mixture was concentrated under reduced pressure, water was added, and the mixture was extracted with toluene. The organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 3.6 g of trifluoroacetaldehyde {2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}hydrazone.

후처리

  1. temperaturewas refluxed
  2. temperaturewith heating for 6 hours
  3. customThe obtained reaction mixture
  4. concentrationwas concentrated under reduced pressure, water
  5. additionwas added
  6. extractionthe mixture was extracted with toluene
  7. washThe organic layer was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-6cb27ba9bd1347ed8de689626fd87816
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07872036B2

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