HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → HCID 58934952, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 69518051 | HCID 69518051 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Acetone cardice | HCID 18522661 | — |
| Product | HCID 58934952 | HCID 58934952 | — |
Reaction Steps
To a solution of 6.8 g (20.6 mmol) of ethyl 6-ethyl-7-methoxy-2-(trifluoromethyl)-2H-chromene-3-carboxylate in 30 mL of anhydrous DCM at −78° C. in dry ice/acetone bath was added dropwise a solution of 206 ml (1.0 M in DCM, 206 mmol) of boron tribromide. After finishing addition, the dry ice/acetone bath was removed. The reaction was stirred at room temperature overnight. The reaction was cooled back to −78° C. in dry ice/acetone bath and treated dropwise with 250 mL of methanol. The reaction was allowed to warm to room temperature and subsequently concd in vacuo. The residue was purified by silica chromatography with EtOAc/hexane (2:8). The collected fractions were concd and used directly in step 3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07259266B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-9a27c31eacec437586966709332ee96f |
| Source note | uspto-grants-2007_08 |