Diethyl Ether → 1-(6,7-Dihydroxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrobromide

HRID 1638791Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1638791
Cl.C([O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20]CC1C=CC=CC=1)[CH2:16][CH2:15][C:14]([C:28]([N:30]1[CH2:35][CH2:34][N:33]([CH2:36][C:37]3[CH:42]=[C:41]([O:43][CH3:44])[C:40]([O:45][CH3:46])=[C:39]([O:47][CH3:48])[CH:38]=3)[CH2:32][CH2:31]1)=[O:29])=[CH:13]2)C1C=CC=CC=1.[BrH:49].C(O)(=O)C.C(OCC)C>C(O)(=O)C>[BrH:49].[OH:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[OH:20])[CH2:16][CH2:15][C:14]([C:28]([N:30]1[CH2:35][CH2:34][N:33]([CH2:36][C:37]3[CH:38]=[C:39]([O:47][CH3:48])[C:40]([O:45][CH3:46])=[C:41]([O:43][CH3:44])[CH:42]=3)[CH2:32][CH2:31]1)=[O:29])=[CH:13]2

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 198411981-(6,7-Dibenzyloxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochlorideHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

Produkt 1

HCID 198412291-(6,7-Dihydroxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrobromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

1-(6,7-dibenzyloxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (0.4 g) is dissolved in acetic acid (8 ml). To the solution is added a 30% solution of hydrogen bromide-acetic acid (4 ml), and the mixture is left standing at room temperature for one hour. To the reaction mixture is added ethyl ether (200 ml), and the mixture is left standing, and then the supernatant is removed by decantation. The precipitates are washed twice with 50 ml each portion of ethyl ether, followed by addition of ethanol (10 ml), whereupon crystallization occurs. The crystals are diluted in ethyl ether (30 ml). The precipitates are collected by filtration to give 1-(6,7-dihydroxy-1,2-dihydro-3-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrobromide (0.25 g) as colorless crystals, m.p. 258°-262° C.

Aufarbeitung

  1. waitthe mixture is left
  2. waitthe mixture is left
  3. customthe supernatant is removed by decantation
  4. washThe precipitates are washed twice with 50 ml each portion of ethyl ether
  5. additionfollowed by addition of ethanol (10 ml), whereupon crystallization
  6. additionThe crystals are diluted in ethyl ether (30 ml)
  7. filtrationThe precipitates are collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-24a5746f539c443899bed6f97e67b2c7
Quelldatensatz
uspto-grants-1989_11
Patentnummer
US04880809

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