Sodium Hypochlorite → HCID 86608017, 화합물

HRID 558618노트

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HRID 558618 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 86608017HCID 86608017, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6422Trifluoroacetic acid용매

실험 절차

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)+].

후처리

  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.]

출처 및 근거

ORD 기록
ord-72ccc341ff3d4f3ba082d56d125191ec
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063048B2

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