Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Acetoxy-2-bromoethane | HCID 13564 | — |
| Reactant | 2,4-Dichloro-6-hydroxybenzaldehyde | HCID 528390 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 89704896 | HCID 89704896 | — |
Reaction Steps
To a solution of 4,6-dichlorosalicylaldehyde (3.72 mmol) in 5 mL DMF was added Cs2CO3 (3.72 mmol) followed by KI (3.72 mmol) and 2-bromoethyl acetate (8.68 mmol). The reaction mixture was heated to 100° C. for 4 h and then stirred at RT for 3 days. The mixture was diluted with EtOAc and washed 3 times with water and then with brine. The combined organic layers were dried over MgSO4 and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using Hept/EtOAc (4/1) to EtOAc gives the desired compound as beige solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09409917B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-0ff5903f7ed74a6498d51455408d3879 |
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| Source note | uspto-grants-2016_08 |
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