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Hydrochloric Acid → Triethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propane-1-sulfonate

HRID 252899
ノート
印刷プレビュー

反応式

HRID 252899 の反応式
[CH2:1]([N:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2].Cl.[F:9][C:10]([F:27])([S:23]([O-:26])(=[O:25])=[O:24])[CH:11]([O:16][C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[C:12]([F:15])([F:14])[F:13].[Na+].ClCCl>O.C(OCC)C>[F:27][C:10]([F:9])([S:23]([O-:26])(=[O:24])=[O:25])[CH:11]([O:16][C:17](=[O:22])[C:18]([CH3:20])([CH3:21])[CH3:19])[C:12]([F:13])([F:15])[F:14].[CH2:1]([NH+:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 8471TriethylamineHCID 86616368Sodium 1,1,3,3,3-Pentafluoro-2-(pivaloyloxy)propane-1-sulfonate

生成物 1

HCID 86618175Triethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propane-1-sulfonate収率 75%

試薬・触媒・溶媒 2

HCID 962
Water
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-(pivaloyloxy)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%. The structure of the obtained product was identified using 1H-NMR, IR and TOFMS spectra.

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-9d821aab383c42b985c8a0ba3e1b29df
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07871761B2

反応ノート

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