Реакция #2016171

Уравнение реакции

19

trans-2,2-dimethyl-propionic acid 3-methyl-piperidin-4-yl ester

L-(−)-0,0′-Dibenzoyl tartaric acid

→

2,2-Dimethyl-propionic acid (3S,4S)-3-methyl-piperidin-4-yl ester

Растворители

EtOAc

EtOAc

Условия реакции

Обработка

1. 1
   ФильтрацияThe formed solid is filtered off
2. 2
   Промывкаwashed with cold EtOAc
3. 3
   Другоеdried
4. 4
   ДругоеIt is then re-crystallized from hot methanol (400 ml)
5. 5
   ДругоеThe crystals are collected
6. 6
   Экстракцияthe free base is liberated by treatment with 1N-NaOH and extraction with ether

Методика

Racemic 19 (62.7 g, 314.4 mmol) is dissolved in EtOAc (300 ml) and a solution of L-(−)-0,0′-Dibenzoyl tartaric acid (56.3 g, 157.2 mmol) in EtOAc (450 ml) is added. The formed solid is filtered off, washed with cold EtOAc and dried. It is then re-crystallized from hot methanol (400 ml). The crystals are collected and the free base is liberated by treatment with 1N-NaOH and extraction with ether.

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