Diethyl Ether → (R)-N-[5-Methyl-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydro-2-naphthyl]-4-morpholinobenzamide Benzenesulfonate

HRID 1862057Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1862057
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[C:8]2[C:3]=1[CH2:4][CH2:5][C@@H:6]([NH:19][C:20](=[O:33])[C:21]1[CH:26]=[CH:25][C:24]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)=[CH:23][CH:22]=1)[CH2:7]2.[C:34]1([S:40]([OH:43])(=[O:42])=[O:41])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.C(OCC)C>O1CCCC1>[C:34]1([S:40]([OH:43])(=[O:42])=[O:41])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.[CH3:1][C:2]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[C:8]2[C:3]=1[CH2:4][CH2:5][C@@H:6]([NH:19][C:20](=[O:33])[C:21]1[CH:26]=[CH:25][C:24]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)=[CH:23][CH:22]=1)[CH2:7]2

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 7371Benzenesulfonic AcidHCID 9846516AR-A000002

Produkt 1

HCID 86584031(R)-N-[5-Methyl-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydro-2-naphthyl]-4-morpholinobenzamide Benzenesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

(R)-N- [5-Methyl-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydro-2-naphthyl]-4-morpholinobenzamide (100 mg, 0.22 mmol) was dissolved in tetrahydrofuran (2 mL) by heating and benzenesulfonic acid (40 mg, 0.24 mmol), dissolved in tetrahydrofuran (4 mL), was added dropwise. Diethyl ether was added and the resulting oil was titurated. The solid was filtered and washed with diethyl ether to give a white solid that was stored in an exicator over blue gel: mp>250° C. Anal. Calcd. for C27H36N4O2×C6H6O3SxH2O: C, 63.4; H, 6.8; N, 9.0. Found: C, 63.1; H, 7.0; N, 8.7.

Aufarbeitung

  1. temperatureby heating
  2. additionwas added dropwise
  3. filtrationThe solid was filtered
  4. washwashed with diethyl ether
  5. customto give a white solid

Quellen und Nachweise

ORD-Eintrag
ord-6bbc804d22ff4d0ca0d9af33fff25e8c
Quelldatensatz
uspto-grants-2003_03
Patentnummer
US06534652B2

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