Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | 15-Crown-5 | HCID 36336 | — |
| Reactant | Sodium Formate | HCID 2723810 | — |
| Reactant | Methyl 4-iodo-3-[2-(3-methyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)-1-propenyloxy]benzoate | HCID 54079273 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 19612294 | HCID 19612294 | — |
Reaction Steps
A mixture of tributylamine (0.4 ml, 0.88 mmol), palladium diacetate (0.017 g, 0.083 mmol), formic acid (0.034 ml, 0.91 mmol), sodium formate (60 mg, 0.88 mmol), 15-crown-5 and methyl 4-iodo-3-[2-(3-methyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)-1-propenyloxy]benzoate (429 mg, 0.83 mmol) in acetonitrile (10 ml) is heated at 45° C. for 8 h. The reaction medium is concentrated on a rotary evaporator under vacuum at 40° C. 20 ml of water and 20 ml of ethyl ether are added. After separation of the phases by settling, the organic phase is washed twice with 20 ml of water, dried over magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05981776 |
|---|
| Source dataset | uspto-grants-1999_11 |
|---|
| ORD ID | ord-a498e0eebd5140eaba7f4d699a7ec314 |
|---|
| Source note | uspto-grants-1999_11 |
|---|