Sodium Iodide → HCID 11514810, Verbindung
Reaktionsgleichung
[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][CH2:12][CH2:13]Cl)[C:7]([O:15][CH3:16])=[CH:6][C:3]=1[C:4]#[N:5].[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.[I-].[Na+]>>[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][CH2:12][CH2:13][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[C:7]([O:15][CH3:16])=[CH:6][C:3]=1[C:4]#[N:5]Komponenten
4
Versuchsvorschrift
A mixture of 2-amino-4-chloropropoxy-5-methoxy-benzonitrile (1.000 g, 4.12 mmol), morpholine (1.0 mL) and catalytic amount of sodium iodide were added into a round bottom flask. The solution was stirred and heated under reflux for 2 h. After reaction, extracted the solution with dichloromethane and water, and then combined the organic phases. After evaporating most of the solvent, equivalent amount of hydrochloric acid ether was added into the solution, and filtered to yield 1.100 g of white solid product with a recovery rate of 91%.
Aufarbeitung
- additionwere added into a round bottom flask
- temperatureheated
- temperatureunder reflux for 2 h
- customAfter reaction
- extractionextracted the solution with dichloromethane and water
- customAfter evaporating most of the solvent, equivalent amount of hydrochloric acid ether
- additionwas added into the solution
- filtrationfiltered
Quellen und Nachweise
- ORD-Eintrag
- ord-ef633660b14c4061a6222317d1f19bf8
- Quelldatensatz
- uspto-grants-2013_01
- Patentnummer
- US08349835B2
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