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

##STR13## In a three necked flask, fitted with a water condenser, a mechanical stirrer and a dropping funnel a solution of 1-bromo-6-cyanohexane (8.04 g, 42.3 mmol) was placed in 75 mL of 95% EtOH. 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 collected by 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. 1H NMR (300 MHz, DMSO-d6) δ 2.50 (t, j=8 Hz, 2H), 2.40(t, 8 Hz, 2H), 1.55 (m, 4H), 1.3(m, 4H).

1. temperatureThe mixture was heated
2. temperatureto reflux and to it
3. temperatureThe mixture was heated for 2 h
4. concentrationconcentrated under reduced pressure
5. dissolutionThe residue was dissolved in 95% EtOH (200 ml)
6. temperatureheated
7. filtrationfiltered
8. concentrationThe filtrate was concentrated
9. temperaturecooled in an ice bath
10. filtrationThe precipitate was collected by filtration
11. customdried

ORDレコード

ord-fcb052a2da6e477a924737dec9203cc3

出典データセット

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05830870