Pyrrolidine → Pyrrolidine, 1-(isocyanoacetyl)-
Reaktionsgleichung
[N+:1]([CH2:3][C:4]([O:6]C)=O)#[C-:2].[NH:8]1[CH2:12][CH2:11][CH2:10][CH2:9]1>>[N+:1]([CH2:3][C:4]([N:8]1[CH2:12][CH2:11][CH2:10][CH2:9]1)=[O:6])#[C-:2]Komponenten
3
Versuchsvorschrift
To stirred and cooled (0° C.) methyl isocyanoacetate (96% technical grade, 5.0 g, 47.8 mmol) was slowly added in 0.75 h pyrrolidine (6.5 mL, 78 mmol). The mixture was stirred for 1.5 h with continued cooling and then concentrated. The resulting oil was co-evaporated twice from CH2Cl2:hexane to remove residual pyrrolidine. 2-Isocyano-1-(pyrrolidin-1-yl)ethanone BLE 04098 was obtained as a yellow solid (6.85 g, 98% yield) and used in the next step without purification.
Aufarbeitung
- stirringThe mixture was stirred for 1.5 h
- temperaturewith continued cooling
- concentrationconcentrated
- customhexane to remove residual pyrrolidine
Quellen und Nachweise
- ORD-Eintrag
- ord-487971cbeee54a0abaa2d7580575f24e
- Quelldatensatz
- uspto-grants-2014_01
- Patentnummer
- US08629165B2
Notizen zur Reaktion
Wird geladen…