Sodium Sulfite → 6-Cyanohexane-l-sulfinic acid sodium salt

In a three necked flask, fitted with a water condenser, a mechanical stirrer and a dropping funnel was placed a solution of 1-bromo-6-cyanohexane (8.04 g, 42.3 mmol) in 75 mL of 95% EtOH was prepared. The mixture was heated to reflux and to it was slowly added a solution of sodium sulfite (8.00 g, 63.5 mmol) in 50 mL of H2O over a period of 30 min. The mixture was heated for 2 h and then concentrated under reduced pressure. The residue was dissolved in 95% EtOH (200 ml), heated to boiling and filtered. The filtrate was concentrated and cooled in an ice bath. The precipitate was collectedby filtration and dried to give 3.00 g of a white solid. The mother liquor on further concentration, produced another batch of 2.2 g of the product.

1. customIn a three necked flask, fitted with a water condenser, a mechanical stirrer and a dropping funnel
2. customwas prepared
3. temperatureThe mixture was heated
4. temperatureto reflux and to it
5. temperatureThe mixture was heated for 2 h
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue was dissolved in 95% EtOH (200 ml)
8. temperatureheated
9. filtrationfiltered
10. concentrationThe filtrate was concentrated
11. temperaturecooled in an ice bath
12. filtrationfiltration
13. customdried

ORD-Eintrag

ord-dd6d62e26be04042bd06b5685fc85da9

Quelldatensatz

uspto-grants-1996_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05550262