Sodium sulfide nonahydrate → 4-(4,4-Difluoro-but-3-enyldisulfanyl)-1,1-difluoro-but-1-ene

HRID 725001

반응식

HRID 725001 반응식
[S-:1][S-:2].[Na+].[Na+].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].[S].Br[CH2:19][CH2:20][CH:21]=[C:22]([F:24])[F:23]>C(O)C>[F:23][C:22]([F:24])=[CH:21][CH2:20][CH2:19][S:1][S:2][CH2:19][CH2:20][CH:21]=[C:22]([F:24])[F:23]

참가 물질

6

반응물 4

HCID 73972Sodium sulfide nonahydrateHCID 89870Sodium disulfideHCID 27822404-Bromo-1,1-difluorobut-1-eneHCID 5362487Sulfur

생성물 1

HCID 217129114-(4,4-Difluoro-but-3-enyldisulfanyl)-1,1-difluoro-but-1-ene

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of sodium disulfide (previously prepared from sodium sulfide nonahydrate (53 g) and sulfur (7.0 g) in ethanol (250 cm3)) was added to 1-bromo4,4-difluorobut-3-ene (50 g) in ethanol (100 cm3). The mixture was gradually heated and stirred under reflux for 2 hours, then cooled and evaporated under reduced pressure. The residue was extracted with diethyl ether, the organic phase filtered to remove sodium bromide and the ether evaporated under reduced pressure to give a liquid which was distilled at 16 mm Hg, bp 120° C. to give the bis-(4,4-difluorobut-3-enyl)disulfide (24 g) as a colourless liquid.

후처리

  1. temperatureThe mixture was gradually heated
  2. temperatureunder reflux for 2 hours
  3. temperaturecooled
  4. customevaporated under reduced pressure
  5. extractionThe residue was extracted with diethyl ether
  6. filtrationthe organic phase filtered
  7. customto remove sodium bromide
  8. customthe ether evaporated under reduced pressure
  9. customto give a liquid which
  10. distillationwas distilled at 16 mm Hg, bp 120° C.

출처 및 근거

ORD 기록
ord-407cb9abcd5e4c0e96152872eb36a75e
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705516

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