Sulfur tetrafluoride → Perfluoro-3-(butoxy)propene

HRID 1680424

反応式

HRID 1680424 の反応式
[F-:1].[K+].[F:3][C:4]([F:15])([C:11]([F:14])([F:13])[F:12])[C:5]([F:10])([F:9])[C:6]([F:8])=[O:7].S(F)(F)(F)F.S(F)(O[C:25]([F:32])([F:31])[C:26]([F:30])=[C:27]([F:29])[F:28])(=O)=O>COCCOCCOC>[F:28][C:27]([F:29])=[C:26]([F:30])[C:25]([F:32])([F:31])[O:7][C:6]([F:1])([F:8])[C:5]([F:10])([F:9])[C:4]([F:15])([F:3])[C:11]([F:12])([F:13])[F:14]

参加物

6

反応物 4

HCID 24555Sulfur tetrafluorideHCID 67632Heptafluorobutyroyl fluorideHCID 522689Potassium FluorideHCID 2776028Pentafluoroallyl fluorosulphate

生成物 1

HCID 54369168Perfluoro-3-(butoxy)propene収率 64%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

反応条件

温度
5 °C

実験手順

A mixture of dry potassium fluoride (7.50 g, 0.13 mol), diglyme (100 ml) and heptafluorobutyroyl fluoride (prepared from the acid by treatment with sulfur tetrafluoride) (28.1 g, 0.13 mol) was stirred at 5° C. for 30 min. Perfluoroallyl fluorosulfate was added dropwise at 5° C., the mixture was stirred at this temperature for 1 hour, then at 25° C. for 3 hours. The volatile components were transferred by distillation at 40° C. (8 mm Hg), washed with water (100 ml), and distilled from a small amount of concentrated sulfuric acid to give perfluoro-3-(butoxy)propene (30.3 g, 0.083 mol, 64%) bp 80°-84° C. whose structure was confirmed by:

後処理

  1. stirringthe mixture was stirred at this temperature for 1 hour
  2. waitat 25° C. for 3 hours
  3. distillationThe volatile components were transferred by distillation at 40° C. (8 mm Hg)
  4. washwashed with water (100 ml)
  5. distillationdistilled from a small amount of concentrated sulfuric acid

出典と根拠

ORDレコード
ord-583dc2b02951406291c442ca2545b358
出典データセット
uspto-grants-1981_06
特許番号
US04273729

関連ノート

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