HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 89618850, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | HCID 131734300 | HCID 131734300 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 89618850 | HCID 89618850 | — |
Reaction Steps
A solution of 2-(6-pivalamidopyridazin-3-yl)acetate (740 mg, 2.52 mmol) in 6 N hydrochloric acid (24 mL) was heated to 105° C. for 12 h, then cooled and concentrated in vacuo. The resulting crude residue was redissolved in methanol (10 mL) and treated dropwise with a 2 N solution of trimethylsilyldiazomethane in diethylether (2.52 mL, 5.04 mmol). After 1 h, the mixture was diluted with water and extracted with EtOAc. The organic layer was washed with water and brine, dried (sodium sulfate), filtered and concentrated to provide title compound. LC-MS (IE, m/z): 168 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09206199B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-b7886ccafb184b74924110e275a9b876 |
| Source note | uspto-grants-2015_12 |