Hydrochloric Acid → HCID 178511248, Verbindung

HRID 50535

Reaktionsgleichung

Reaktionsgleichung von HRID 50535
C(OC(=O)[NH:7][CH2:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][NH:16][S:17]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH:23]=[CH:22][CH:21]=2)(=[O:19])=[O:18])[CH2:11][CH2:10]1)(C)(C)C.Cl>C(Cl)(Cl)Cl.O1CCOCC1>[NH2:7][CH2:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][NH:16][S:17]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH:23]=[CH:22][CH:21]=2)(=[O:19])=[O:18])[CH2:11][CH2:10]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 178453605HCID 178453605, Verbindung

Produkt 1

HCID 178511248HCID 178511248, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A suspension of trans-{4-[(naphthalene-1-sulfonylamino)-methyl]-cyclohexylmethyl}-carbamic acid tert-butyl ester (25 g) in chloroform (300 ml) is treated with a 4 N HCl solution in dioxane (300 ml) at 0° C. After completion, the reaction mixture is concentrated in vacuo, the residue is taken up in a 1 N sodium hydroxide solution and dichloromethane. After extraction with dichloromethane, the organics are dried over sodium sulfate and concentrated to 18.5 g of trans-naphthalene-1-sulfonic acid (4-aminomethyl-cyclohexylmethyl) -amide as a white powder melting at 157-162° C. Rf(C3) 0.36.

Aufarbeitung

  1. concentrationAfter completion, the reaction mixture is concentrated in vacuo
  2. extractionAfter extraction with dichloromethane
  3. dry with materialthe organics are dried over sodium sulfate
  4. concentrationconcentrated to 18.5 g of trans-naphthalene-1-sulfonic acid (4-aminomethyl-cyclohexylmethyl) -amide as a white powder melting at 157-162° C

Quellen und Nachweise

ORD-Eintrag
ord-1876bdd7156e49868d7a80f5dfff8d30
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06713265B1

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