Tripropylamine → 4-Chloro-1-methylquinazolin-2(1H)-one

A mixture of 1-methylquinazoline-2,4-dione (8.8 g), tri-n-propylamine (8.6 g) and phosphorus oxychloride (80 ml) was stirred for 1 hour at 110°-120° C. The resultant mixture was cooled to ambient temperature and concentrated under reduced pressure to give a residue, which was dissolved in 2% tri-n-propylamine-chloroform solution. The solution was added dropwise to a mixture of 2 N sodium hydroxide aqueous solution and ice at alkaline pH. The aqueous layer was separated and extracted twice with chloroform. The combined chloroform layer was washed with water and with aqueous solution saturated with sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give crystalline 4-chloro-1-methyl-1H-quinazoline-2-one.

1. concentrationconcentrated under reduced pressure
2. customto give a residue, which
3. customThe aqueous layer was separated
4. extractionextracted twice with chloroform
5. washThe combined chloroform layer was washed with water and with aqueous solution saturated with sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-17061e7924be45d094b08c59460e6e0b

Quelldatensatz

uspto-grants-1984_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04429126