Hydrochloric Acid → Triethylammonium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate

HRID 252900

反応式

HRID 252900 の反応式
[CH2:1]([N:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2].Cl.[F:9][C:10]([F:29])([S:25]([O-:28])(=[O:27])=[O:26])[CH:11]([O:16][C:17](=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]([F:15])([F:14])[F:13].[Na+].ClCCl>O.C(OCC)C>[F:29][C:10]([F:9])([S:25]([O-:28])(=[O:26])=[O:27])[CH:11]([O:16][C:17](=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]([F:13])([F:15])[F:14].[CH2:1]([NH+:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 8471TriethylamineHCID 58112889Sodium 2-benzoyloxy-1,1,3,3,3-pentafluoropropanesulfonate

生成物 1

HCID 86618176Triethylammonium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate収率 75%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

Triethylamine was dissolved in cold water, and hydrochloric acid was added thereto to adjust the pH of the reaction liquid to fall within a range of 1 to 3. Then sodium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate and dichloromethane were added thereto and stirred. The separated organic layer was washed with water, and dichloromethane was removed under reduced pressure from the washed organic layer. To the residue thus obtained, diethyl ether was added for recrystallization. The resultant was filtrated and dried to obtain a desired product at a yield of 75%.

後処理

  1. customthe pH of the reaction liquid
  2. washThe separated organic layer was washed with water, and dichloromethane
  3. customwas removed under reduced pressure from the washed organic layer
  4. customTo the residue thus obtained
  5. filtrationThe resultant was filtrated
  6. customdried

出典と根拠

ORDレコード
ord-9c58d534780a4f299c49d84e8b761102
出典データセット
uspto-grants-2011_01
特許番号
US07871761B2

関連ノート

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