HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Bromo-2-methyl-1-propene → HCID 178441184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Bromo-2-methyl-1-propene | HCID 357785 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Reactant | HCID 178518180 | HCID 178518180 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178441184 | HCID 178441184 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
To the mixture of 2-((1S,2S,4R)-bicyclo[2.2.1]heptan-2-ylamino)-5-(2-(tetrahydro-2H-pyran-2-yloxy)ethyl)thiazol-4(5H)-one (1160 mg, 3.43 mmol) in THF (8.0 mL) cooled in a −78° C. bath was added LDA (2.0 M, 17.15 mL). The resulting mixture was stirred for 10 min at −78° C., and then 3-bromo-2-methylprop-1-ene (1.6 ml, 17.15 mmol) was added. After the reaction mixture was allowed to warm to room temperature and stirred ca. 18 h. Saturated NaH2PO4 was added, and the aqueous phase was extracted with EtOAc. The organic layer was washed with sat'd NH4Cl, dried over MgSO4, filtered, and concentrated in vacuo. The crude residue was purified by flash chromatography (4:1; Hexane:EtOAc) to give the title compound as yellow oil. MS (ES+): 393 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08686011B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-b7dd2c3c2757432280f485cab6696c81 |
| Source note | uspto-grants-2014_04 |