HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 10012348, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | 2,2,3,3-Tetramethylcyclopropane-1-carbonyl chloride | HCID 11041002 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10012348 | HCID 10012348 | 75% |
Reaction Steps
Tetramethylcyclopropanecarbonyl chloride (TMC-Cl) (4 g; 25 mmol) dissolved in 20 ml of dry dichloromethane was slowly added to a stirred and dry dichloromethane solution of methoxylamine hydrochloride (2.5 g; 30 mmol) and triethylamine (6.3 g; 50 mmol). After the addition, the reaction mixture was stirred for 2 hr at room temperature. Dichloromethane was evaporated under vacuum, 10 ml of water was added and the products were extracted using 30 ml of ethyl acetate. The organic fraction was dried over MgSO4, filtered and evaporated under vacuum. The product was crystallized using 20 ml ethyl acetate and 30 ml petroleum ether to afford 3 g (75% yield) and its chemical structure was identified by elemental analysis and spectroscopic methods.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07232929B2 |
| Source dataset | uspto-grants-2007_06 |
| ORD ID | ord-112bfaf24afb4065964848a4ef512747 |
| Source note | uspto-grants-2007_06 |