Hydrochloric Acid → HCID 54096058, compound

A 200 ml flask equipped with a mechanical stirrer, condenser, thermometer and heating mantle was charged with iron powder (26.0 g, 464 mmol) and 30 ml of water. This mixture was heated on a steam bath for 30 minutes. Concentrated hydrochloric acid (7 ml) and 4-butenyloxynitrobenzene (14.0 g, 72 mmol) were added dropwise simultaneously. After the addition was complete, the reaction mixture was stirred on a steam bath for an additional four hours. The reaction mixture was quenched by slowly adding a solution of sodium hydroxide (7.0 g, 175 mmol) in 15 ml of water and it was filtered hot. The filtrate was washed twice with 100 ml of hot benzene. The organic layers were combined, dried (MgSO4), and filtered. Solvent was removed under reduced pressure and the product was vacuum dried for three hours at 50° C. and 0.8mm/Hg. Yield=4.0g (34%).

1. customA 200 ml flask equipped with a mechanical stirrer, condenser
2. temperaturethermometer and heating mantle
3. temperatureThis mixture was heated on a steam bath for 30 minutes
4. additionAfter the addition
5. customThe reaction mixture was quenched
6. filtrationwas filtered hot
7. washThe filtrate was washed twice with 100 ml of hot benzene
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customSolvent was removed under reduced pressure
11. customdried for three hours at 50° C.

ORD record

ord-6d5b3558e74240c49b2ff0cc21b09666

Source dataset

uspto-grants-1989_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04806608