Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,2-dichloro-1,1,2-trifluoro-4-iodobutane | HCID 4712671 | — |
| Reactant | Methyl 2-(3,3,3-trifluoropropylsulfonyl)acetate | HCID 57425720 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 59370911 | HCID 59370911 | 22.4% |
Reaction Steps
To a solution of 5.0 g of 1,2-dichloro-1,1,2-trifluoro-4-iodobutane and 3.8 g of methyl (3,3,3-trifluoropropylsulfonyl)acetate in 100 ml of dimethyl sulfoxide was added 0.7 g of sodium hydride (60% in oil) at room temperature, and the mixture was stirred at the same temperature for 3 days. To the reaction mixture was added 10% hydrochloric acid, and then extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was subjected to silica gel chromatography to obtain 1.50 g of methyl 5,6-dichloro-5,6,6-trifluoro-2-(3,3,3-trifluoropropylsulfonyl)hexanoate (hereinafter referred to as the present compound (1)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08158829B2 |
|---|
| Source dataset | uspto-grants-2012_04 |
|---|
| ORD ID | ord-0796ee2d2527497084644a92362b99b3 |
|---|
| Source note | uspto-grants-2012_04 |
|---|