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Hydrochloric Acid → HCID 23373708, Verbindung

HRID 865935
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 865935
[CH3:1][CH:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]2[CH:19]=[C:20]([CH:29]=[CH:30][CH:31]=2)[C:21]([N:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)=O)[CH2:13][CH2:12]1)[CH3:3].C1(C)C=CC=CC=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:48]2)=CC=1.[OH-].[Na+].[ClH:63]>>[ClH:63].[CH3:1][CH:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]2[CH:19]=[C:20]([CH:29]=[CH:30][CH:31]=2)[C:21]([N:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)=[S:48])[CH2:13][CH2:12]1)[CH3:3]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 313Hydrochloric AcidHCID 1140Toluene2×HCID 14798Sodium HydroxideHCID 60820MazapertineHCID 87949Lawesson's reagent

Produkt 1

HCID 23373708HCID 23373708, Verbindung

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A solution of 1-[3-[[4-[2-(1-methylethoxy)phenyl]-1-piperazinyl]methyl]benzoyl]piperidine (CP #36, 3.86 g, 0.0092 mol) and toluene (50 mL) was treated with 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (2.22 g, 0.0055 mole) and the resulting mixture was heated at 90° C. for 1 h. The reaction was cooled followed by the addition of toluene (50 mL), and mixed thoroughly with excess 3N sodium hydroxide solution. The organic layer was separated, washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated to an oily residue. Chromatography of this material on flash silica, using 1.5-2.5% methanol in methylene chloride, afforded CP #1 which was converted to its hydrochloride salt in ethereal hydrochloric acid, 3.61 g (77%), m.p. 221°-224° C. (dec, uncorrected). The structural assignment was supported by 1H NMR, chemical-ionization MS, and IR data.

Aufarbeitung

  1. temperatureThe reaction was cooled
  2. customThe organic layer was separated
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated to an oily residue
  6. customafforded CP #1 which

Quellen und Nachweise

ORD-Eintrag
ord-c4ef0384909445058f2a58f98d104018
Quelldatensatz
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05569659

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