HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 57803565, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 69054868 | HCID 69054868 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57803565 | HCID 57803565 | — |
Reaction Steps
6-Methoxymethoxy-5,7,8-trimethyl-2,3-dihydro-4H-thiochromen-4-one (23 mg) was dissolved in anhydrous DMF (5 mL) and treated with 1,2-dichloroethane (6.8 μL) and NaH (60% in mineral oil, 8.2 mg), and stirred for 19 h at ambient temperature. The reaction mixture was poured into H2O and extracted with EtOAc. The organic layer was collected and dried over Na2SO4 followed by solvent evaporation. Column chromatography (SiO2: hexane:EtOAc, from 9:1 to 1:1 v/v) yielded a fraction containing impure desired product 6-methoxymethoxy-5,7,8-trimethyl-2,3-dihydro-4H-thiochromen-4-one (<1 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07576094B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-49e07af7b85f412090ddcad2b0d33d18 |
| Source note | uspto-grants-2009_08 |