HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 21162713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | Sodium methanesulfinate | HCID 2733271 | — |
| Reactant | Methyl 11-hydroxy-6,11-dihydrobenzo[c][1]benzoxepine-2-carboxylate | HCID 2769059 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21162713 | HCID 21162713 | 68.6% |
Reaction Steps
Reflux 1.4 gm. of methyl 6,11-dihydro-11-hydroxydibenz[b,e]oxepin-2-carboxylate in 6 cc. of thionyl chloride for 10 minutes. Strip away excess thionyl chloride by evaporation and dissolve the chloro intermediate so produced in 14 cc. of N,N-dimethylformamide. Add 582 mg. of methanesulfinic acid sodium salt (10% excess). Stir at room temperature for 5 days. Dilute with water and separate the solids by filtration. Crystallize from 15 cc. of benzene to obtain the title product (yield 1.18 gm. 68.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04282365 |
| Source dataset | uspto-grants-1981_08 |
| ORD ID | ord-1c9ffca1b4cc4110bc7077c60b236f4f |
| Source note | uspto-grants-1981_08 |