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

HRID 589541ノート

反応式

HRID 589541 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-d06013dbc7c945378785e8474decb2c2
出典データセット
uspto-grants-2016_01
特許番号
US09233919B2

反応ノート

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