Potassium Hydroxide → HCID 86620368、化合物

HRID 1725322ノート

反応式

HRID 1725322 の反応式
[I:1][C:2]([F:18])([F:17])[C:3]([F:16])([F:15])[O:4][C:5]([F:14])([F:13])[C:6]([F:12])([F:11])[S:7](F)(=[O:9])=[O:8].[OH-].[K+].C1C[O:24]CC1.O.[Br-].[C:28]1([S+:34]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>O.C(Cl)Cl>[I:1][C:2]([F:18])([F:17])[C:3]([F:16])([F:15])[O:4][C:5]([F:14])([F:13])[C:6]([F:12])([F:11])[S:7]([O-:24])(=[O:9])=[O:8].[C:41]1([S+:34]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1

参加物

7

反応物 4

HCID 14797Potassium HydroxideHCID 27751695-Iodoperfluoro-3-oxapentanesulfonyl fluorideHCID 11984010Triphenylsulfonium BromideHCID 21881883Oxolane--water (1/1)

生成物 1

HCID 86620368HCID 86620368、化合物収率 82%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

12.56 grams (0.03 mol) of 5-iodooctafluoro-3-oxapentanesulfonyl fluoride (Synquest) was taken in a flask in water and excess amount of KOH (0.06 mol, 3.31 grams) was added and the resulting mixture was heated under stirring at 80° C. for six hours. To this reaction mixture (after cooling to room temperature) was added 1:2 v/v THF/water solution of triphenyl sulfonium bromide (0.03 mol, 10.14 grams) dropwise over a period of one hour with stirring. After the addition, the reaction mixture was further stirred for additional 3 hours at room temperature. Upon completion, the target compound triphenylsulfonium 5-iodooctafluoro-3-oxapentafluoro sulfonate was extracted using methylene chloride. It was washed at least three times with DI water. Methylene chloride was evaporated to get a pale yellow liquid. It was redissolved in methylene chloride and precipitated into hexanes. Yield was 82%. Melting point (capillary) 110-112° C.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureTo this reaction mixture (after cooling to room temperature)
  3. stirringwith stirring
  4. additionAfter the addition
  5. stirringthe reaction mixture was further stirred for additional 3 hours at room temperature
  6. extractionUpon completion, the target compound triphenylsulfonium 5-iodooctafluoro-3-oxapentafluoro sulfonate was extracted
  7. washIt was washed at least three times with DI water
  8. customMethylene chloride was evaporated
  9. customto get a pale yellow liquid
  10. customprecipitated into hexanes
  11. customMelting point (capillary) 110-112° C.

出典と根拠

ORDレコード
ord-84d9d3b3d36c46828b892b4b5f965918
出典データセット
uspto-grants-2009_02
特許番号
US07491482B2

反応ノート

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