HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 2-(3-Cyclopropylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Diiodomethane | HCID 6346 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 2-(3-Ethenylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 22240170 | — |
| Reactant | HCID 178418750 | HCID 178418750 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(3-Cyclopropylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 22240222 | 10% |
Reaction Steps
To a solution of Zn(C2H5)2 (1 M, 6 mL) in DCM (1 mL) was added trifluoro-acetic acid (0.46 ml, 6 mmol) in DCM (1 mL) very slowly under N2 in ice bath. The mixture was stirred for 20 minutes. CH2I2 (1.61 g, 6 mmol) in DCM (1 mL) was added to the mixture. After stirring for 20 minutes, 4,4,5,5-tetramethyl-2-(3-vinylphenyl)-1,3,2-dioxaborolane (690 mg, 3 mmol) in DCM (1 mL) was added. The mixture was stirred at room temperature for 2 hour. the mixture was quenched by NH4Cl solution, extracted with DCM 3 times, washed with brine, filtered and concentrated to give the residue, which was purified preparative TLC and HPLC to give 2-(3-cyclopropylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (70 mg, 10%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450308B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-35b21563b998431697a124af13ebbb41 |
| Source note | uspto-grants-2013_05 |