HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 5-(Tert-butyldimethylsilanyloxy)-5-(1-propylcyclobutyl)pent-2-en-1-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | tert-Butyl-[4-iodo-1-(Propylcyclobutyl)but-3-enyloxy]dimethylsilane | HCID 53961856 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Pentane | HCID 8003 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-(Tert-butyldimethylsilanyloxy)-5-(1-propylcyclobutyl)pent-2-en-1-ol | HCID 67102120 | 33% |
Reaction Steps
tert-Butyllithium (1.32 mL of a 1.7M solution in pentane, 2.25 mmol) was added to a solution of the vinyl iodide 6 (460 mg, 1.25 mmol) in THF (2.2 mL) at −78° C. After 0.5 h paraformaldehyde (50 mg, 1.67 mmol) was added. The reaction was warmed to room temperature and stirred for 16 h. The reaction was quenched with saturated aqueous NH4Cl and extracted with EtOAc. The organic portion was dried (MgSO4), filtered and concentrated in vacuo. FCC (silica gel, 4:1 hex/EtOAc) yielded 103 mg (33%) of the alcohol 7 as a clear, colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07314890B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-daadba8693b64f99a3c95729daec8390 |
| Source note | uspto-grants-2008_01 |