Reaktion #81525

Reaktionsgleichung

[1-[2-[(Methylsulphonyl)amino]ethyl]-4-piperidinyl]methyl[2-(3-methyl-1,2,4-oxadiazol-5-yl)phenyl]carbamate

maleic acid

→

title compound

Ausbeute 88.3%

[1-[2-[(Methylsulphonyl)amino]ethyl]-4-piperidinyl]methyl[2-(3-methyl-1,2,4-oxadiazol-5-yl)phenyl]carbamate (Z)-2-butenedioate

Ausbeute 88.3%

Lösungsmittel

methanol dichloromethane

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe resultant solution was concentrated in vacuo
2. 2
   Sonstigeto give a viscous gum which
3. 3
   SonstigeThe beige solid was crystallised from absolute ethanol (500 ml)

Vorschrift

[1-[2-[(Methylsulphonyl)amino]ethyl]-4-piperidinyl]methyl[2-(3-methyl-1,2,4-oxadiazol-5-yl)phenyl]carbamate (11.83 g) was dissolved in warm methanol/dichloromethane (50 ml/25 ml) and treated with a warm solution of maleic acid (2.91 g) in methanol (25 ml). The resultant solution was concentrated in vacuo to give a viscous gum which rapidly solidified upon standing. The beige solid was crystallised from absolute ethanol (500 ml) to give the title compound (12.25 g) as fluffy white microneedles, m.p. 163°-164°.

Quelle