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Hydrochloric Acid → HCID 86736579, Verbindung

HRID 2058968
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2058968
[O:1]1[CH:7]2[CH:2]1[CH2:3][N:4]([C:8]([O:10][CH2:11][C:12]([Cl:15])([Cl:14])[Cl:13])=[O:9])[CH2:5][CH2:6]2.[ClH:16]>O1CCOCC1.O>[OH:1][C@H:2]1[C@H:7]([Cl:16])[CH2:6][CH2:5][N:4]([C:8]([O:10][CH2:11][C:12]([Cl:15])([Cl:14])[Cl:13])=[O:9])[CH2:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 20548869HCID 20548869, Verbindung

Produkt 1

HCID 86736579HCID 86736579, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

5.0 g (0.018 mol) of 3,4-epoxy-1-(β,β,β-trichloroethoxycarbonyl)-piperidine are dissolved in 50 ml of dioxane and the solution is treated with 60 ml of 6 N hydrochloric acid. The slightly exothermic reaction is kept at room temperature by means of a water bath, and the reaction mixture is stirred for 15 hours, then diluted with water and extracted with 3 times 100 ml of methylene chloride. The organic phase is washed with 0.1 N sodium hydroxide solution and then with a saturated aqueous solution of sodium chloride, dried over sodium sulphate and then evaporated to dryness, first under a water pump vacuum and then under a high vacuum, whereupon trans-3-hydroxy-4-chloro-1-(β,β,β-trichloroethoxycarbonyl)-piperidine is obtained in the form of a slightly yellow oil.

Aufarbeitung

  1. customThe slightly exothermic reaction
  2. customis kept at room temperature by means of a water bath
  3. extractionextracted with 3 times 100 ml of methylene chloride
  4. washThe organic phase is washed with 0.1 N sodium hydroxide solution
  5. dry with materialwith a saturated aqueous solution of sodium chloride, dried over sodium sulphate
  6. customevaporated to dryness, first under a water pump vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a55f62f1abc84a10a917ff89756d08ec
Quelldatensatz
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04320137

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