Water → 1-(2,4-Dichlorophenyl)-3-hydroxyurea

Temperatur

25 °C

A solution of 14.2 g (75 mmol) of 2,4-dichlorophenylisocyanate in 50 mL of toluene was added to a mixture of 8.26 g (120 mmol) of hydroxylamine hydrochloride and 4.8 g (120 mmol) of sodium hydroxide in a two-phase solvent mixture consisting of 50 mL of water and 50 mL of toluene. The resulting mixture was stirred at 25° C. for 30 minutes and filtered. The solid thus obtained was washed with water and then dissolved in 200 mL of ethyl acetate. The solution was dried over magnesium sulfate and the solvent was removed under reduced pressure to yield 12.7 g of the title compound of Step A as a white solid melting at 157-158° C. It was used directly in the next step without further purification.

1. filtrationfiltered
2. customThe solid thus obtained
3. washwas washed with water
4. dissolutiondissolved in 200 mL of ethyl acetate
5. dry with materialThe solution was dried over magnesium sulfate
6. customthe solvent was removed under reduced pressure

ORD-Eintrag

ord-cd4a5e9706a14379bd3486860ef85942

Quelldatensatz

uspto-grants-2004_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06737383B1