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Hydrochloric Acid → HCID 13851158, Verbindung

HRID 978481
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 978481
[ClH:1].[C:2]1([CH:8]2[O:13][CH2:12][CH2:11][NH:10][CH2:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:14]([CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27](=O)[CH3:28])=[CH:22][CH:21]=1)([O:16][CH3:17])=[O:15].C([BH3-])#N.[Na+].Cl>CO.ClCCl.C(OCC)C>[ClH:1].[CH3:17][O:16][C:14](=[O:15])[CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][CH:27]([N:10]2[CH2:11][CH2:12][O:13][CH:8]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9]2)[CH3:28])=[CH:22][CH:21]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 123435392-Phenylmorpholine hydrochlorideHCID 13851156Methyl 2-(4-(2-oxopropyl)phenoxy)acetate

Produkt 1

HCID 13851158HCID 13851158, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887
Methanol
Lösungsmittel
2×
HCID 3283Diethyl EtherLösungsmittel
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2-phenylmorpholine hydrochloride (6.05 g), 1-(4-carbomethoxymethoxyphenyl)propan-2-one (6.63 g) and sodium cyanoborohydride (1.61 g) in methanol (100 ml) was stirred at room temperature for 22 hours. The solvent was removed under reduced pressure and aqueous sodium bicarbonate solution added to the residue and extracted with dichloromethane (X2). The extracts were washed with aqueous sodium bicarbonate, dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated to dryness to give an oil. Chromatography on silica gel in 0→7% methanol in dichloromethane gave an oil which was dissolved in diethyl ether and treated with an ethereal solution of hydrogen chloride. Evaporation to dryness and trituration of the residue with ethyl acetate gave a solid. Recrystallisation of this solid gave the title compound, m.p. 187°-190° C. (methanol-ethyl acetate), of analytical purity.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure and aqueous sodium bicarbonate solution
  2. additionadded to the residue
  3. extractionextracted with dichloromethane (X2)
  4. washThe extracts were washed with aqueous sodium bicarbonate
  5. dry with materialdried over anhydrous magnesium sulphate
  6. filtrationfiltered
  7. customthe filtrate evaporated to dryness
  8. customto give an oil
  9. customEvaporation to dryness and trituration of the residue with ethyl acetate
  10. customgave a solid
  11. customRecrystallisation of this solid

Quellen und Nachweise

ORD-Eintrag
ord-05b5a75635e641588194fdb9daef7f58
Quelldatensatz
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04665072

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