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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
ノート
印刷プレビュー

反応式

HRID 253321 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6cb27ba9bd1347ed8de689626fd87816
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07872036B2

反応ノート

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