Sodium Hypochlorite → HCID 86608017、化合物

HRID 1293727ノート

反応式

HRID 1293727 の反応式
[CH2:1]([S:3][C:4](SCC)=[C:5]([C:19]([F:22])([F:21])[F:20])[CH2:6][C:7]([C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=1)=[O:8])[CH3:2].[O-:26]Cl.[Na+]>C(O)(C(F)(F)F)=O.O>[CH2:1]([S:3][C:4](=[O:26])[CH:5]([C:19]([F:22])([F:21])[F:20])[CH2:6][C:7](=[O:8])[C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=1)[CH3:2]

参加物

5

反応物 2

HCID 23665760Sodium HypochloriteHCID 866080184,4-Bis-ethylsulfanyl-3-trifluoromethyl-1-(4-trifluoromethyl-phenyl)-but-3-en-1-one

生成物 1

HCID 86608017HCID 86608017、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A mixture of 4,4-bis-ethylsulfanyl-3-trifluoromethyl-1-(4-trifluoromethyl-phenyl)-but-3-en-1-one (example C.26 step 3) (36.96 g, 92 mmol) in TFA (54.3 mL) and water (5.8 mL) was refluxed for 18 h under nitrogen atmosphere, the exhaust of the reaction was passed through a NaOCl solution to trap the liberated ethyl mercaptane. The volatiles were evaporated and the mixture was diluted with water and extracted with TBME, the organic layer was washed with sat. NaHCO3-sol. and brine, dried over Na2SO4. Removal of the solvent in vacuum left the title compound as a brown oil (31.2 g, 95%), which was used without further purification [according to J. Fluorine Chem. 2001, 107, 281.]. MS (EI) 339.0 [(M−F)+].

後処理

  1. temperaturewas refluxed for 18 h under nitrogen atmosphere
  2. customThe volatiles were evaporated
  3. additionthe mixture was diluted with water
  4. extractionextracted with TBME
  5. washthe organic layer was washed with sat. NaHCO3-sol
  6. dry with materialand brine, dried over Na2SO4
  7. customRemoval of the solvent in vacuum
  8. waitleft the title compound as a brown oil (31.2 g, 95%), which
  9. customwas used without further purification [according to J. Fluorine Chem. 2001, 107, 281.]

出典と根拠

ORDレコード
ord-7f82045526df4bd68c14d687d833cf70
出典データセット
uspto-grants-2007_07
特許番号
US07238808B2

反応ノート

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