Hydrochloric Acid → HCID 54478463, compound

To a suspension of 1-methyl-2-nitroisourea (1.5 g) in water (15 ml), methylamine hydrochloride (0.9 g) was added (pH: 3.3). An aqueous sodium hydroxide (1%) was gradually added to maintain the pH of the suspension at 8 at room temperature. After the suspension was stirred for 3 hours at room temperature while maintaining the pH thereof to 8, 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 by silica gel column chromatography (hexane/ethyl acetate: 2/1) and then recrystallized (ethyl acetate-hexane), to obtain the desired compound (1.0 g) as colorless crystals.

1. additionwas added (pH: 3.3)
2. temperaturewhile maintaining the pH
3. extractionthe solution was extracted with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate, and it
6. concentrationwas then concentrated under reduced pressure
7. customThe residual oil was purified by silica gel column chromatography (hexane/ethyl acetate: 2/1)
8. customrecrystallized (ethyl acetate-hexane)

ORD record

ord-73d580956be14d4e922b301316093def

Source dataset

uspto-grants-2000_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06124466