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Hydrochloric Acid → HCID 20489855, Verbindung

HRID 1701180
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1701180
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].C1(C2[NH:24][CH2:23][CH:22]([CH2:25][Cl:26])[O:21]2)C=CC=CC=1.Cl>C(Cl)(Cl)Cl.N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6]([NH:24][CH2:23][CH:22]([OH:21])[CH2:25][Cl:26])=[O:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 77070Veratroyl chlorideHCID 2707015-(Chloromethyl)-2-phenyl-1,3-oxazolidine

Produkt 1

HCID 20489855HCID 20489855, VerbindungAusbeute 72,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittel
HCID 6212
Chloroform
Lösungsmittel
2×

Versuchsvorschrift

A solution of 15.2 g of 3,4-dimethoxybenzoyl chloride in 40 ml of chloroform is added dropwise to a solution of 15.0 g 2-phenyl-5-chloromethyloxazolidine in a mixture of 200 ml of chloroform and 6 ml of pyridine at a temperature of -40° C. under agitation. This solution is then heated to room temperature. After a reaction period of 14 hours, 20 ml of concentrated hydrochloric acid are added, the phases are thoroughly mixed for a period of 10 minutes and then are separated. The separated aqueous phase is diluted with water to twice its volume and then is saturated with sodium chloride and extracted with chloroform. After drying the chloroform-extract and evaporating the solvent, 15.0 g of N-(3,4-dimethoxybenzoyl)-3-chloro-1-aminopropan-2-ol is obtained as an oil which can be further reacted without any purification. After crystallization from ethanol/toluene the compound exhibits a melting point of 104°-106° C.

Aufarbeitung

  1. additionare added
  2. additionthe phases are thoroughly mixed for a period of 10 minutes
  3. customare separated
  4. additionThe separated aqueous phase is diluted with water to twice its volume
  5. extractionextracted with chloroform
  6. dry with materialAfter drying the chloroform-
  7. extractionextract
  8. customevaporating the solvent

Quellen und Nachweise

ORD-Eintrag
ord-63524c6d042b45f0a959b571a658f3e8
Quelldatensatz
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04191770

Notizen zur Reaktion

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