Formaldehyde → (R)-Methyl 1-methylpyrrolidine-2-carboxylate
Reaktionsgleichung
[CH3:1][O:2][C:3](=[O:9])[C@H:4]1[CH2:8][CH2:7][CH2:6][NH:5]1.[CH2:10]=O>CN(C=O)C>[CH3:1][O:2][C:3](=[O:9])[C@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[CH3:10]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
(2R)-proline methylester (1.20 g, 10.0 mmol) was dissolve in DMF (30 mL), and formalin (37% in water, 1.12 mL, 15.0 mmol) and NaBH (OAc)3 (4.20 g, 20.0 mmol) were added portionwise. After 12 h, the reaction material was concentrated in vacuo, and the residue was diluted with NaHCO3 (30 mL). The organic material was extracted with EtOAc, and the organic extracts were dried over MgSO4 and concentrated in vacuo. The residue was purified by column chomatography (EtOAc/Hex=4/1) to give the title compound (1.33 g, 93.0%).
Aufarbeitung
- concentrationthe reaction material was concentrated in vacuo
- additionthe residue was diluted with NaHCO3 (30 mL)
- extractionThe organic material was extracted with EtOAc
- dry with materialthe organic extracts were dried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by column chomatography (EtOAc/Hex=4/1)
Quellen und Nachweise
- ORD-Eintrag
- ord-eb3a8e91ebaa468084ee19832f0d7f82
- Quelldatensatz
- uspto-grants-2011_08
- Patentnummer
- US07989634B2
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