Hydrochloric Acid → HCID 45263090, Verbindung

HRID 27246Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 27246
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:23][CH2:22][C:21]2[C:16](=[C:17]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=[CH:19][CH:20]=2)[C:15]1=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[Na+].[ClH:33]>CCOCC.O.O1CCCC1>[ClH:33].[CH2:7]([N:14]1[CH2:23][CH2:22][C:21]2[C:16](=[C:17]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=[CH:19][CH:20]=2)[CH2:15]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 233443172-Benzyl-8-phenyl-3,4-dihydroisoquinolin-1(2H)-one

Produkt 1

HCID 45263090HCID 45263090, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

3.6 Parts of lithium aluminum hydride is added to a solution of 10 parts of 2-benzyl-3,4-dihydro-8-phenyl-1(2H)-isoquinolone in 225 parts by volume dry tetrahydrofuran and the resulting mixture is stirred at reflux temperature for about 5 hours. Then the mixture is cooled in an ice bath and treated successively with 7.5 parts by volume of water in 15 parts by volume of tetrahydrofuran, 7.5 parts by volume of 25% sodium hydroxide, and 7.5 parts by volume of water. The salts which form are filtered off and the filtrate is dried over anhydrous magnesium sulfate and concentrated under reduced pressure to yield clear oil. The oil is taken up in ether and treated with isopropanolic hydrogen chloride to give, as a white solid, 2-benzyl-8-phenyl-1,2,3,4-tetrahydroisoquinoline hydrochloride, melting at about 187°-189° C. after recrystallization from a mixture of ethanol and ether. This compound has the following formula ##STR16##

Aufarbeitung

  1. temperatureat reflux temperature for about 5 hours
  2. temperatureThen the mixture is cooled in an ice bath
  3. filtrationThe salts which form are filtered off
  4. dry with materialthe filtrate is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto yield clear oil

Quellen und Nachweise

ORD-Eintrag
ord-4ce3cf20126c41bb873dee78da9b6aa0
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04220778

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