1,1-Bis(2,2-dimethylpropoxy)-N,N-dimethylmethanamine → HCID 20491764, Verbindung

Temperatur

90 °C

N,N-Dimethylformamide dineopentyl acetal (1.8 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (522 mg) and 2-hydroxymethyl-5-methylfuran (628 mg) in dry N,N-dimethylformamide (10 ml) under nitrogen. The resulting solution was then stirred and heated at 90° C. under nitrogen. After 1.5 h the reaction mixture was evaporated to a brown crystalline solid (1.030 g). The solid was subjected to column chromatography on silica (70-230 mesh) (100 g) developing with chloroform-ethanol, 29:1. The resulting pale yellow solid (327 mg) was crystallised twice from acetone to give white needles of the title furan (206 mg), m.p. 166°-167° C., λmax 226 nm (ε 15,660), 332 nm (ε 2,520), λinf 247 nm (ε 3,100).

1. customAfter 1.5 h the reaction mixture was evaporated to a brown crystalline solid (1.030 g)
2. customThe resulting pale yellow solid (327 mg) was crystallised twice from acetone

ORD-Eintrag

ord-3c111c8bccee427da371b6fea9153b0e

Quelldatensatz

uspto-grants-1983_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04399140