HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 4-(Tert-butyl-dimethyl-silanyloxy)-2-isopropyl-benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | (4-Bromo-3-isopropyl-phenoxy)-tert-butyl-dimethyl-silane | HCID 22568908 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pentane | HCID 8003 | — |
| Product | 4-(Tert-butyl-dimethyl-silanyloxy)-2-isopropyl-benzaldehyde | HCID 22568900 | 55.1% |
Reaction Steps
A solution of (4-bromo-3-isopropyl-phenoxy)-tert-butyl-dimethyl-silane (Intermediate 145, 1.03 g, 3.13 mmols) in 25 mL E2O was cooled to −78° C. and treated with tert-butyllithium (401.0 mg, 6.26 mmols; 3.7 mL of a 1.7M solution in pentane). After 30 minutes the reaction was quenched with DMF (913.0 mg, 12.5 mmols) and warmed to room temperature. The solution was diluted with H2O, extracted with Et2O and the combined organic layers washed with H2O and saturated aqueous NaCl before being dried (MgSO4) and concentrated under reduced pressure. Column chromatography (2% EtOAc-hexanes) afforded 480.0 mg (55%) of the title compound as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06399774B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-a865b08b801742ce835fd52aa61ddbd0 |
| Source note | uspto-grants-2002_06 |