2-Chloropropane → 4-Methyl-1,1,1-trifluoro-2-trifluoromethyl-2,3-pentane diol

HRID 252689

Reaktionsgleichung

Reaktionsgleichung von HRID 252689
[Mg].[CH:2](Cl)([CH3:4])[CH3:3].[OH:6][C:7]([C:16]([F:19])([F:18])[F:17])([C:12]([F:15])([F:14])[F:13])[C:8](OC)=[O:9].[Cl-].[NH4+]>O1CCCC1>[CH3:3][CH:2]([CH3:4])[CH:8]([OH:9])[C:7]([C:12]([F:13])([F:14])[F:15])([OH:6])[C:16]([F:19])([F:18])[F:17]

Komponenten

6

Edukt 4

HCID 63612-ChloropropaneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 9877912Methyl 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropionate

Produkt 1

HCID 594588154-Methyl-1,1,1-trifluoro-2-trifluoromethyl-2,3-pentane diolAusbeute 84,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A flask was charged with 9.5 g of magnesium and 300 ml of tetrahydrofuran, to which 35.0 g of isopropyl chloride was added dropwise at 50° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 20.2 g of the target compound (yield 84%).

Aufarbeitung

  1. additionwas added dropwise at 50° C
  2. additionAfter the completion of dropwise addition
  3. stirringThe mixture was stirred for one hour at room temperature
  4. distillationThis was followed by ordinary work-up and vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-b726f97347004953aa51b1eebbc904b3
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07868199B2

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