反応 #81525

反応方程式

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

maleic acid

→

title compound

収率 88.3%

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

収率 88.3%

溶媒

methanol dichloromethane

methanol

反応条件

後処理

1. 1
   濃縮The resultant solution was concentrated in vacuo
2. 2
   その他to give a viscous gum which
3. 3
   その他The beige solid was crystallised from absolute ethanol (500 ml)

実験手順

[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°.

出典