Hydrochloric Acid → alpha-(3,4-Dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride

HRID 66323Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 66323
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]1[CH2:11][O:10]1.[CH3:12][O:13][C:14]1[CH:15]=[C:16]([CH:20]=[CH:21][C:22]=1[O:23][CH3:24])[CH2:17][CH2:18][NH2:19].C(Cl)(Cl)[Cl:26].Cl>C(O)C.C(OCC)C>[ClH:26].[CH3:12][O:13][C:14]1[CH:15]=[C:16]([CH:20]=[CH:21][C:22]=1[O:23][CH3:24])[CH2:17][CH2:18][NH:19][CH2:11][CH:9]([OH:10])[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[O:2][CH3:1]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 8421HomoveratrylamineHCID 113555722-(2-Methoxyphenyl)oxirane

Produkt 1

HCID 22754925alpha-(3,4-Dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of 0.5 g of 2-(2-methoxyphenyl)oxirane (crude product) and 600 mg of 3,4-dimethoxyphenethylamine is heated at 130° to 140° C. for 2 hours. After cooling, chloroform is added to the reaction mixture, and said mixture is washed with water. The mixture is dried and evaporated to remove solvent. 2 ml of ethanol are added to the residue obtained. Then, hydrochloric acid-containing diethylether is added to the ethanol mixture, and crystalline precipitates are collected by filtration. 290 mg of α-(3,4-dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride are obtained as crystals. M.p. 142°-143° C.

Aufarbeitung

  1. temperatureis heated at 130° to 140° C. for 2 hours
  2. temperatureAfter cooling
  3. washis washed with water
  4. customThe mixture is dried
  5. customevaporated
  6. customto remove solvent
  7. addition2 ml of ethanol are added to the residue
  8. customobtained
  9. customcrystalline precipitates
  10. filtrationare collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-3c46bf617041418a86107e3f0c445eca
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04131686

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