Formic Acid → HCID 178467450, Verbindung
Reaktionsgleichung
ClC1C=CN=NN=1.Cl[C:9]1[N:14]=[C:13]([O:15][CH2:16][CH3:17])[N:12]=[C:11]([N:18]([CH3:20])[CH3:19])[N:10]=1.C(O)=[O:22]>>[CH3:19][N:18]([CH3:20])[C:11]1[N:12]=[C:13]([O:15][CH2:16][CH3:17])[NH:14][C:9](=[O:22])[N:10]=1Komponenten
4
Versuchsvorschrift
The chlorotriazine from (b) (1.2 g.) was heated in formic acid (15 ml.) on a steam bath for 45 minutes, when gas evolution had ceased. The excess of formic acid was removed under reduced pressure and the residue was dissolved in the minimum amount of water, which was brought to pH 6-7 by adding solid sodium bicarbonate. The solution was extracted with chloroform and the extracts dried and evaporated. The residue crystallised from ethanol to give the product (1.1 g.) having a melting point of 215°-216° C. (The melting point sample resolidified and re-melted at 235° C.).
Aufarbeitung
- customThe excess of formic acid was removed under reduced pressure
- dissolutionthe residue was dissolved in the minimum amount of water, which
- additionby adding solid sodium bicarbonate
- extractionThe solution was extracted with chloroform
- customthe extracts dried
- customevaporated
- customThe residue crystallised from ethanol
- customto give the product (1.1 g.)
Quellen und Nachweise
- ORD-Eintrag
- ord-2aba6e9fea4b4dd4b164cd99b70f5199
- Quelldatensatz
- uspto-grants-1980_10
- Patentnummer
- US04226990
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