p-Toluenesulfonic acid → HCID 19937311, Verbindung

HRID 36589Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 36589
[F:1][C:2]([F:23])([CH2:11][N:12]1[C:16](=[O:17])[C:15]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:14]2[C:13]1=[O:22])[CH2:3][O:4]C1CCCCO1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[F:23][C:2]([F:1])([CH2:11][N:12]1[C:16](=[O:17])[C:15]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:14]2[C:13]1=[O:22])[CH2:3][OH:4]

Komponenten

4

Edukt 2

HCID 6101p-Toluenesulfonic acidHCID 19937334HCID 19937334, Verbindung

Produkt 1

HCID 19937311HCID 19937311, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2,2-difluoro-3-phthalimido-1-tetrahydropyranyloxypropane (2 g, 6.15 mmol), paratoluene sulfonic acid (0.1 g) in absolute ethanol was stirred overnight at room temperature. Then the mixture was concentrated in vacuo, diluted with ethyl acetate and .,washed with brine. The organic phase was separated, dried over magnesium sulfate and concentrated in vacuo. The crude alcohol 2,2-difluoro-3-phthalimido-1-propanol (1.4 g) was used for the next step without further purification.

Aufarbeitung

  1. concentrationThen the mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. customThe organic phase was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude alcohol 2,2-difluoro-3-phthalimido-1-propanol (1.4 g) was used for the next step without further purification

Quellen und Nachweise

ORD-Eintrag
ord-6e5d03d2f4b843e893a93aa80a544745
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05416076

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