Trifluoroacetic acid → 2,2-Bis(trifluoromethyl)-4-carbamoyloxymethyl-1,3-dioxolane

HRID 1439525Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1439525
[F:1][C:2]([F:15])([F:14])[C:3]1([C:10]([F:13])([F:12])[F:11])[O:7][CH:6]([CH2:8][OH:9])[CH2:5][O:4]1.[O:16]([C:18]#[N:19])[Na].FC(F)(F)C(O)=O>C(Cl)Cl>[F:13][C:10]([F:11])([F:12])[C:3]1([C:2]([F:1])([F:14])[F:15])[O:7][CH:6]([CH2:8][O:9][C:18](=[O:16])[NH2:19])[CH2:5][O:4]1

Komponenten

5

Edukt 3

HCID 6422Trifluoroacetic acidHCID 219971032,2-Bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolaneHCID 178418852HCID 178418852, Verbindung

Produkt 1

HCID 213957942,2-Bis(trifluoromethyl)-4-carbamoyloxymethyl-1,3-dioxolane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A mixture of 15 grams of 2,2-bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane (0.0625 mols), 8.12 grams NaOCN (0.125 mols), and 75 ml methylene dichloride is stirred at 25°-35° C. while 14.3 grams trifluoroacetic acid is added dropwise. The mixture is stirred for 16 hours at 40° C. The product is filtered and the filter cake washed with methylene dichloride. The filtrate is washed with water and dried over Na2SO4 prior to vacuum-stripping. The reaction product is recrystallized from 1 part benzene to yield 2,2-bis(trifluoromethyl)-4-carbamoyloxymethyl-1,3-dioxolane (m.p. 52°-54° C.)

Aufarbeitung

  1. additionis added dropwise
  2. filtrationThe product is filtered
  3. washthe filter cake washed with methylene dichloride
  4. washThe filtrate is washed with water
  5. dry with materialdried over Na2SO4
  6. customThe reaction product is recrystallized from 1 part benzene

Quellen und Nachweise

ORD-Eintrag
ord-c4e22f8cc72b48549b5b2f044ce78e8e
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04060532

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