Formaldehyde → HCID 23084733, compound

Temperature

60 °C

While heating a mixture of dimethylamine hydrochloride (2.45 g) and 37% aqueous formalin solution (2.43 g) to 50° C., acetic anhydride (9.4 mL) was added dropwise thereto slowly. After the completion of the dropwise addition, the mixture was heated at 60° C. for 30 min. 3-Isopropyl-2H-isoquinolin-1-one (1.87 g) was added, and the mixture was stirred with heating at 80-100° C. for 1 day. After the completion of the reaction, the solvent was evaporated. The obtained residue was dissolved in 1N hydrochloric acid, and the mixture was washed with chloroform. Aqueous potassium carbonate solution was added to alkalify the aqueous layer, and the mixture was extracted with chloroform, and the organic layer was dried over magnesium sulfate. The solvent was evaporated, and the obtained residue was purified by silica gel column chromatography (chloroform:methanol=30:1) to give 4-dimethylaminomethyl-3-isopropyl-2H-isoquinolin-1-one (0.39 g).

1. temperatureWhile heating
2. additionAfter the completion of the dropwise addition
3. temperaturewith heating at 80-100° C. for 1 day
4. customAfter the completion of the reaction
5. customthe solvent was evaporated
6. dissolutionThe obtained residue was dissolved in 1N hydrochloric acid
7. washthe mixture was washed with chloroform
8. additionAqueous potassium carbonate solution was added
9. extractionthe mixture was extracted with chloroform
10. dry with materialthe organic layer was dried over magnesium sulfate
11. customThe solvent was evaporated
12. customthe obtained residue was purified by silica gel column chromatography (chloroform:methanol=30:1)

ORD record

ord-208a136c94274b2092f67b3ffbd33b59

Source dataset

uspto-grants-2009_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07501412B2