HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 10203615, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1,1,1-Trifluoro-2-iodoethane | HCID 67709 | — |
| Reactant | HCID 10155312 | HCID 10155312 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10203615 | HCID 10203615 | 48.7% |
Reaction Steps
The product of Example 63 (100 mg, 0.28 mmol) was dissolved in anhydrous DMF (3 mL) and treated with 1,1,1-trifluoro-2-iodoethane (27.5 mL, 280 mmol) in presence of anhydrous sodium carbonate (130 mg, 1.2 mmol) at 50–60° C. for 2 hours. The reaction mixture was partitioned between water and ethyl acetate to provide the desired compound as an amorphous solid (60 mg, 48%). 1HNMR (300 MHz, CDCl3) δ 2.10 (s, 3H), 3.10 (s, 3H), 4.85 (q, J=9 Hz, 2H), 6.90 (m, 2H), 7.10 (dd, J=6 Hz, J=9 Hz, 2H), 7.25 (m, 2H), 7.95 (d, J=9 Hz, 2H). MS (DCI/NH3) 458 (M+NH4)+ Anal. calc. for C20H16N2F4SO3: C, 54.54; H, 3.66; N, 6.36. Found: C, 54.41; H, 3.56; N, 6.35.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115591B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-fad5c5515f9a426cb6e5ea2f4c240b33 |
| Source note | uspto-grants-2006_10 |