methyl 4-amino-2-methoxycyclohexane-1-carboxylate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 4-(benzylamino)-2-methoxycyclohexanecarboxylate (1.84 g, 6.63 mmol, racemic mixture of diastereomers) and palladium hydroxide on carbon (20 weight %, 0.233 g, 0.332 mmol) in methanol (35 mL) were combined, and the atmosphere was exchanged for hydrogen (balloon) via four vacuum hydrogen flush cycles. After 24 hours, additional palladium hydroxide on carbon (20 weight %, 0.233 g, 0.332 mmol) was added, and the reaction mixture was again placed under a hydrogen atmosphere. Following another 24 hours, the reaction mixture was filtered through diatomaceous earth and concentrated under reduced pressure to give methyl 4-amino-2-methoxycyclohexanecarboxylate as a racemic mixture of three diastereomers, which was carried forward without further purification. MS ESI calcd. for C9H18NO3 [M+H]+ 188. found 188. flush cycles Following another 24 hours the reaction mixture was filtered through diatomaceous earth concentrated under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 4-(benzylamino)-2-methoxycyclohexanecarboxylate (1.84 g, 6.63 mmol, racemic mixture of diastereomers) and palladium hydroxide on carbon (20 weight %, 0.233 g, 0.332 mmol) in methanol (35 mL) were combined, and the atmosphere was exchanged for hydrogen (balloon) via four vacuum hydrogen flush cycles. After 24 hours, additional palladium hydroxide on carbon (20 weight %, 0.233 g, 0.332 mmol) was added, and the reaction mixture was again placed under a hydrogen atmosphere. Following another 24 hours, the reaction mixture was filtered through diatomaceous earth and concentrated under reduced pressure to give methyl 4-amino-2-methoxycyclohexanecarboxylate as a racemic mixture of three diastereomers, which was carried forward without further purification. MS ESI calcd. for C9H18NO3 [M+H]+ 188. found 188. flush cycles Following another 24 hours the reaction mixture was filtered through diatomaceous earth concentrated under reduced pressure