HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → Tert-butyl 2-(2-bromo-4-formylphenoxy)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 3-Bromo-4-hydroxybenzaldehyde | HCID 76308 | — |
| Reactant | tert-Butyl bromoacetate | HCID 79177 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Tert-butyl 2-(2-bromo-4-formylphenoxy)acetate | HCID 17999215 | 98.4% |
Reaction Steps
To a solution of 3-bromo-4-hydroxybenzaldehyde (5 g, 25 mmol, 1 eq, Aldrich, Milwaukee, Wis., USA) in DMF (200 mL) was added solid cesium carbonate (16.25 g, 50 mmol, 2 eq) followed by dropwise addition of t-butyl 2-bromoacetate (4.4 mL, 30 mmol, 1.2 eq, Aldrich, Milwaukee, Wis., USA). After stirring at room temperature for 18 h, the DMF was removed in vacuo and the resultant residue was extracted between EtOAc (50 mL) and brine (50 mL). The separated organic layer was dried (Na2SO4), and concentrated in vacuo to give 7.74 g (98.4%) of t-butyl 2-(2-bromo-4-formylphenoxy)acetate (1). 1HNMR (CDCl3, 300 MHz): δ 9.83 (s, 1H), 8.08 (d, 1H), 7.76 (dd, 1H), 6.83 (d, 1H), 4.67 (s, 1H).1.44 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822467B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-03cdefa305c4419ab250d0cc1ffdea8f |
| Source note | uspto-grants-2014_09 |