Methanesulfonic Acid → HCID 19968402, Verbindung

HRID 975834Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 975834
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1>CCOCC>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 10220867HCID 10220867, Verbindung

Produkt 1

HCID 19968402HCID 19968402, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of methanesulphonic acid (0.3 g) in ether (15 ml) was added dropwise to a cooled solution of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene (0.8 g, prepared in a similar manner to that described in Example 14) in ether (25 ml). The resulting solid was collected by filtration, washed with ether and dried in vacuo at ambient temperature to yield 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene methanesulphonate as a white solid. Yield 1.0 g, mp 226°-231.5° C.

Aufarbeitung

  1. customprepared in a similar manner to that
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with ether
  4. customdried in vacuo at ambient temperature

Quellen und Nachweise

ORD-Eintrag
ord-d9b7f9ce48f04b17b2fb4d4107a9b341
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05610161

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