HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 86659919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 73443586 | HCID 73443586 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 86659919 | HCID 86659919 | — |
Reaction Steps
To a solution of isochroman-3,4-dione 4-oxime (98% pure, 3.5 g, 0.02 mol) in methanol (35 g) and dichlormethane (32 g) was added dropwise at 20-30° C. thionyl chloride (24.0 g, 0.2 mol). The resulting mixture was stirred at ambient temperature for 3 d. The reaction was monitored by HPLC. After completion of the reaction, the mixture was concentrated in vacuo and a crude residue was obtained (5.5 g). A part of this residue (5.1 g) was dissolved in MTBE and was washed with water. The mixture was concentrated and the resulting residue was purified by silica column chromatography by yield (2-chloromethyl-phenyl)-hydroxyimino-acetic acid methyl ester as a colorless solid (3.4
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575366B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-844661f778dc4730b15d14db45322966 |
| Source note | uspto-grants-2013_11 |