HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 10815838, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Benzoic acid, 4-(cyanomethyl)-2-ethoxy-, ethyl ester | HCID 10489807 | — |
| Reactant | HCID 54424526 | HCID 54424526 | — |
| Solvent | 1,2-Dichlorobenzene | HCID 7239 | — |
| Product | HCID 10815838 | HCID 10815838 | — |
Reaction Steps
At 23-25° C., a solution of ethyl 2-ethoxy-4-cyanomethyl-benzoate (2.35 g, 10 mmol) and α-cyclohexylmethyl-2-piperidino-benzyl alcohol(2.88 g, 10 mmol) in o-dichlorobenzene (15 ml) is added dropwise to a mixture of concentrated sulphuric acid (15 ml) and o-dichlorobenzene (15 ml). The mixture is stirred for 2 hours at ambient temperature. The o-dichlorobenzene phase is then separated off and the residue is added to ice. After being made alkaline with soda solution, it is extracted with chloroform. The extracts are dried over sodium sulphate and concentrated by evaporation. The residue is purified by column chromatography on silica gel (toluene/acetone=10/1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06143769 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-fdc29c0be4fc4621bf299119242b67ac |
| Source note | uspto-grants-2000_11 |