HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide → 3-(3,5-Dichloro-2-aminophenyl)-5,6-dihydro-1,4,2-dioxazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide | HCID 86630772 | — |
| Solvent | Thionyl Chloride | HCID 24386 | — |
| Product | 3-(3,5-Dichloro-2-aminophenyl)-5,6-dihydro-1,4,2-dioxazine | HCID 57731173 | — |
Reaction Steps
At 20° C., 30 ml of thionyl chloride are initially charged and 3 g of 3,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide are added in 3 portions with stirring. The mixture is stirred at 70° C. for 12 h. The reaction mixture is then cooled and carefully poured onto ice-water. The mixture is extracted twice with in each case 150 ml of dichloromethane and the extracts are dried with sodium sulphate and evaporated to dryness using a rotary evaporator.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08486934B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-2ac7fc0a7d7b49cc8a9b0c5fa36cd912 |
| Source note | uspto-grants-2013_07 |