Sodium Bicarbonate → HCID 178527275, Verbindung

HRID 1711422Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1711422
[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([O:14][C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[C:17]([CH2:22][S:23]([C:26]3[C:35]4[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=4)[CH:29]=[CH:28][CH:27]=3)(=[O:25])=[O:24])[CH:16]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:36]([O-])=O.[Na+].C(=O)(O)[O-].[Na+]>C1COCC1.Cl.O>[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([O:14][C:15]2[CH:16]=[C:17]3[C:18](=[CH:19][CH:20]=2)[NH:21][N:36]=[C:22]3[S:23]([C:26]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH:29]=[CH:28][CH:27]=2)(=[O:25])=[O:24])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

7

Edukt 3

HCID 516892Sodium BicarbonateHCID 23668193Sodium NitriteHCID 588286234-(1-Benzylpiperidin-3-yloxy)-2-(1-naphthylsulfonylmethyl)phenylamine

Produkt 1

HCID 178527275HCID 178527275, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 4-(1-benzylpiperidin-3-yloxy)-2-(1-naphthylsulfonylmethyl)phenylamine (1.0 g, 2 mmoles) in THF and 4M HCl (10 mL), under nitrogen, at 3° C. was treated dropwise with a solution of sodium nitrite (0.16 g, 2.4 mmoles) in H2O, poured into a cold solution of saturated sodium bicarbonate and extracted with EtOAc. The extracts were combined, dried over Na2SO4, and concentrated under vacuum to afford the title compound as an off white solid (0.7 g, 1.4 mmoles).

Aufarbeitung

  1. extractionextracted with EtOAc
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-137168122da04461a5803aaf6be7fd70
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07790751B2

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