HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12851303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl 4-piperidinecarboxylate | HCID 70770 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12851303 | HCID 12851303 | 94.6% |
Reaction Steps
To a solution of 76.5 g of ethyl isonipecotate and 81.5 ml of triethylamine in 750 ml of methylene chloride, 149 g of triphenylmethyl chloride dividied in three portions was added portionwise at room temperature, and the mixture was stirred for 16 hours. The reaction mixture was added with water and extracted with methylene chloride. The extract was washed successively with water and saturated brine, and dried, and then the solvent was evaporated. The resulting brown liquid was added with diisopropyl ether, and the precipitated crystals were collected by filtration and washed with diisopropyl ether to give 184 g of pale yellow crystals. Recrystallization from ethanol gave colorless prisms having the melting point of from 147.5 to 148.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06518265B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-24546867800b414abe166b49cf748b80 |
| Source note | uspto-grants-2003_02 |