Toluene → Sodium 2-benzoyloxy-1,1,3,3,3-pentafluoropropanesulfonate

HRID 2074055

反応式

HRID 2074055 の反応式
[C:1]([O:9][C:10]([C:14]([F:17])([F:16])[F:15])=[C:11]([F:13])[F:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:18]([O-:21])([OH:20])=[O:19].[Na+:22].C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C1(C)C=CC=CC=1>O>[F:13][C:11]([F:12])([S:18]([O-:21])(=[O:20])=[O:19])[CH:10]([O:9][C:1](=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:14]([F:16])([F:15])[F:17].[Na+:22]

参加物

6

反応物 4

HCID 1140TolueneHCID 7187Benzoyl PeroxideHCID 2782398Pentafluoroprop-1-en-2-yl benzoateHCID 23665763Sodium Bisulfite

生成物 1

HCID 58112889Sodium 2-benzoyloxy-1,1,3,3,3-pentafluoropropanesulfonate収率 43%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

10.0 g of 1,1,3,3,3-pentafluoropropen-2-yl benzoate which had been synthesized by a conventional technique, was dispersed in 72 g of water, after which 12.0 g of sodium hydrogen sulfite and 1.24 g of benzoyl peroxide were added. Reaction occurred at 85° C. for 65 hours. The reaction solution was allowed to cool, after which toluene was added, followed by separatory operation to separate a water layer. A saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals settled out. The crystals were collected by filtration, washed with a small volume of saturated sodium chloride aqueous solution and then dried in vacuum, obtaining the target compound, sodium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate. White crystals, 5.85 g (yield 43%).

後処理

  1. customReaction
  2. temperatureto cool
  3. customto separate a water layer
  4. additionA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
  5. filtrationThe crystals were collected by filtration
  6. washwashed with a small volume of saturated sodium chloride aqueous solution
  7. customdried in vacuum

出典と根拠

ORDレコード
ord-9103bfa7028849b1a9c2e5d4579bdca4
出典データセット
uspto-grants-2011_04
特許番号
US07919226B2

関連ノート

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