Hydrochloric Acid → RS 93007

HRID 65308

Reaktionsgleichung

Reaktionsgleichung von HRID 65308
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35].CCOCC>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 1291023-(4-Cyano-4-(3,4-dimethoxyphenyl)-5-methylhex-1-yl)-1,2,3,4-tetrahydro-6,7-dimethoxy-2-methylisoquinoline

Produkt 1

HCID 129101RS 93007

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel2×

Versuchsvorschrift

The free base, 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline (1, 15 g, 0.032 mol) was dissolved in isopropanol (70 mL) at 70° C., and 6M HCl in isopropanol (5.6 mL) slowly added. After cooling to room temperature, ether (40 mL) was added until the solution became cloudy (saturated), and the resulting mixture stirred overnight. The resulting solid was collected, washed thoroughly with ether-isopropanol (1:1, 50 mL), and dried in vacuo at 50° C. to yield 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline·HCl (1·HCl, 13.7 g, m.p. 115°-120° C.) as a white powder.

Aufarbeitung

  1. customThe resulting solid was collected
  2. washwashed thoroughly with ether-isopropanol (1:1, 50 mL)
  3. customdried in vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-f7b0d798c79c4e5d88ee89341c0c7a36
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04613606

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