Hydrochloric Acid → Benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate

HRID 1625641노트

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HRID 1625641 반응식
[F:1][C:2]([F:19])([S:15]([O-:18])(=[O:17])=[O:16])[CH:3]([O:8]C(=O)C(C)(C)C)[C:4]([F:7])([F:6])[F:5].[CH2:20]([N+:27]([CH3:30])([CH3:29])[CH3:28])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[OH-].[Na+].Cl>CO.O>[F:19][C:2]([F:1])([S:15]([O-:18])(=[O:16])=[O:17])[CH:3]([OH:8])[C:4]([F:5])([F:7])[F:6].[CH2:20]([N+:27]([CH3:30])([CH3:29])[CH3:28])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86665356Benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-pivaloyloxypropane-1-sulfonate

생성물 1

HCID 86664292Benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate수율 98%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

In 139 g of methanol was dissolved 46.3 g (0.1 mole) of benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-pivaloyloxypropane-1-sulfonate in Synthesis Example 2. The solution was stirred under ice cooling, to which a solution of 8.0 g (0.2 mole) of sodium hydroxide in 24 g of water was added dropwise at a temperature below 20° C. The solution was stirred overnight at room temperature, after which 21 g of conc. hydrochloric acid and 60 g of water were added to quench the reaction. Methanol was removed in vacuum from the reaction solution, dichloromethane and water were added to the residue, and the organic layer was separated and concentrated again. To the residue containing some white crystals, 150 g of diisopropyl ether was added for crystallization. Filtration and drying gave the target compound. White crystals, 37 g, yield 98%.

후처리

  1. customin Synthesis Example 2
  2. additionwas added dropwise at a temperature below 20° C
  3. customto quench
  4. customthe reaction
  5. customMethanol was removed in vacuum from the reaction solution, dichloromethane and water
  6. additionwere added to the residue
  7. customthe organic layer was separated
  8. concentrationconcentrated again
  9. additionTo the residue containing some white crystals, 150 g of diisopropyl ether
  10. additionwas added for crystallization
  11. filtrationFiltration
  12. customdrying
  13. customgave the target compound

출처 및 근거

ORD 기록
ord-0a42af4c78974c2cb34a42c704e07180
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785105B2

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