Hydrochloric Acid → HCID 54478463, compound

To a suspension of 1-methyl-2-nitroisourea (1.0 g) in a buffer solution of a tris(hydroxymethyl)aminomethanehydrochloric acid (tris-hydrochloric acid buffer solution, 1.0 M, pH: 7.5, 10 ml), methylamine hydrochloride (0.6 g) was added at room temperature. After stirring for 3 hours, an aqueous hydrochloric acid (4 M) was added, and then the solution was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, and it was then concentrated under reduced pressure. The residual oil was purified with silica gel column chromatography (hexane/ethyl acetate: 2/1) and then recrystallized (ethyl acetate-hexane), to obtain the desired compound (0.8 g) as colorless crystals.

1. additionwas added at room temperature
2. extractionthe solution was extracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate, and it
5. concentrationwas then concentrated under reduced pressure
6. customThe residual oil was purified with silica gel column chromatography (hexane/ethyl acetate: 2/1)
7. customrecrystallized (ethyl acetate-hexane)

ORD record

ord-5f96dd2e53a049b893c270c56e2bb157

Source dataset

uspto-grants-2000_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06124466