Hydrochloric Acid → HCID 13006892, Verbindung

A 7.9 g (0.092 mole) portion of 2-imidazolidinone in 92 ml of dimethylsulfoxide was treated with 12.7 g (0.092 mole) of K2CO3, 7.4 g (0.045 mole) of potassium iodide and 20.0 g (0.092 mole) of 2-hydroxy-5-nitrobenzyl bromide. The reaction mixture was heated to 105° over 0.3 hours and held at 105° for 1.6 hours. The reaction mixture was poured with stirring into 550 ml of water. The aqueous mixture was acidified with 9 ml of concentrated HCl and extracted with 480 ml of chloroform. The chloroform extract was washed with 60 ml of H2O, dried over MgSO4 overnight and filtered. The filtrate was concentrated under reduced pressure to give 18 g of a yellow semi-solid. The crude product was crystallized using 65 ml of benzene and filtered, washing with ether to give 9.7 g (44%) of a light yellow semi-solid. Recrystallization from acetonitrile gave an analytical sample, m.p. 222°-224° dec.

1. temperatureThe reaction mixture was heated to 105° over 0.3 hours
2. additionThe reaction mixture was poured
3. extractionextracted with 480 ml of chloroform
4. extractionThe chloroform extract
5. washwas washed with 60 ml of H2O
6. dry with materialdried over MgSO4 overnight
7. filtrationfiltered
8. concentrationThe filtrate was concentrated under reduced pressure

ORD-Eintrag

ord-68b133b975dd448389ab1c8fc39c6058

Quelldatensatz

uspto-grants-1976_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US03932452