Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | HCID 13250834 | HCID 13250834 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86642967 | HCID 86642967 | — |
Reaction Steps
To a suspension of 15.10 g of a double salt of 2KHSO5.KHSO4.K2SO4 (Oxone, registered trade mark) in 100 ml of water was added dropwise a solution of 4.77 g of (3,3,4,4,5,5,6,6,6-nonafluorohexylthio)acetonitrile in 100 ml of methanol at −20° C. over 60 minutes under a nitrogen atmosphere, and the mixture was stirred for 2 hours. To the reaction mixture was added 50 ml of an aqueous 10% sodium sulfite solution, followed by extraction with 100 ml of ethyl acetate twice. Organic layers were combined, washed with 50 ml of an aqueous 10% sodium sulfite solution and 50 ml of an aqueous saturated sodium chloride solution, dried over sodium sulfate, filtered, and then concentrated under rescued pressure. The residue was subjected to silica gel column chromatography to obtain 12.56 g of (3,3,4,4,5,5,6,6,6-nonafluorohexylsulfinyl)acetonitrile represented by the formula:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08247596B2 |
|---|
| Source dataset | uspto-grants-2012_08 |
|---|
| ORD ID | ord-4acc3ccdf05543389f5db8dbf015c22d |
|---|
| Source note | uspto-grants-2012_08 |
|---|