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

HRID 650615

反応式

HRID 650615 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-3475dfc603334e56b64100cc5912dc74
出典データセット
uspto-grants-2001_08
特許番号
US06274632B1

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