HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86756990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrile | HCID 93865 | — |
| Reactant | HCID 10219671 | HCID 10219671 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86756990 | HCID 86756990 | 46.4% |
Reaction Steps
A solution of Example 1C (2.68 g, 12.5 mmol), triethylamine (3.47 ml, 75.0 mmol), and 2-(tert-butyoxycarbonyloxyimino)-2-phenylacetonitrile (3.22 g, 13.0 mmol) in 30% aqueous dioxane was heated to 50° C. for 6 hours, cooled to ambient temperature, and concentrated. The residue was diluted with aqueous sodium hydroxide (0.25M, 50 mL) and extracted twice with ethyl acetate. The aqueous layer was acidified to pH 3 with 1M H3PO4 and extracted five times with chloroform. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated to provide the desired product (1.62 g). MS (ESI) m/e 278 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07030262B2 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-edc47b4aa4dc4bc49395d706e44a2e60 |
| Source note | uspto-grants-2006_04 |