HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 50915499, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,1,1-Trifluoro-4-iodobutane | HCID 2775189 | — |
| Reactant | HCID 50915333 | HCID 50915333 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 50915499 | HCID 50915499 | 67% |
Reaction Steps
Compound 45 is prepared following synthesis method 6: 0.3 g (0.7 mmol) of intermediate 7b are placed in 10 mL DMF in the presence of 0.13 g (0.94 mmol) K2CO3 then 0.222 g (0.90 mmol) of 1,1,1-trifluoro-4-iodo-butane and agitated at 80° C. for 32 h. After concentrating to dryness, the residue is solubilized in water and extracted with AcOEt. The organic phases are washed in brine, dried over Na2SO4 then concentrated to dryness. The residue is purified by silica gel flash chromatography (gradient CH2Cl2-MeOH: 100:0 to 99:1 for 30 nm). 0.250 g of compound 45 are collected (yield: 67%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946225B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-02f97cc921ef43fba0ccd8d3eb3a1f36 |
| Source note | uspto-grants-2015_02 |