Butyl Acrylate → HCID 86644274, compound

Temperature

120 °C

A 0.28 mM palladium acetate solution (3.28 ml) was added to N-methylpyrrolidone (7 ml) solution of 2-bromo-5-nitrotoluene (1 g) and sodium acetate trihydrate (417 mg) in an argon atmosphere. The mixture was warmed to 120° C., and n-butyl acrylate (923 μl) was added thereto. The obtained mixture was stirred at 135° C. for 2 hours. A 0.28 mM palladium acetate solution (3.28 ml) and n-butyl acrylate (396 μl) were further added thereto, and the mixture was stirred for 4 hours. Subsequently, sodium acetate (265 mg) was added, and the mixture was further stirred for 1 hour. After the reaction was over, water (30 ml) was added to the resulting reaction mixture, and the mixture was separated with toluene and water. The organic layer was washed three times with water and once with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. After the solvent was distilled off, the obtained residue was isolated and purified by silica gel column chromatography (n-hexane to ethyl acetate=8:1) to obtain Compound 5a (1.05 g, 86%).

1. stirringthe mixture was stirred for 4 hours
2. stirringthe mixture was further stirred for 1 hour
3. additionwas added to the resulting reaction mixture
4. customthe mixture was separated with toluene and water
5. washThe organic layer was washed three times with water
6. dry with materialonce with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate
7. distillationAfter the solvent was distilled off
8. customthe obtained residue was isolated
9. custompurified by silica gel column chromatography (n-hexane to ethyl acetate=8:1)

ORD record

ord-95fff439bbee4f868eed69082349cf50

Source dataset

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07855300B2