HuagongsheHuagongshe Chemistry Print Report · For research reference only
Butylamine → 2,4-Bis-benzyloxy-5-isopropenyl-benzoic acid benzyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Butylamine | HCID 8007 | — |
| Reactant | Benzyl-2,4-bis-benzyloxy-5-bromobenzoate | HCID 46915635 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Propan-2-ol--water (1/1) | HCID 21889133 | — |
| Product | 2,4-Bis-benzyloxy-5-isopropenyl-benzoic acid benzyl ester | HCID 59263118 | 119.5% |
Reaction Steps
A mixture of 2,4-bis-benzyloxy-5-bromo-benzoic acid benzyl ester (10.0 g, 20 mmol), potassium isopropenyl trifluoroborate (4.0 g, 27.2 mmol) and n-butylamine (6.0 mL, 60 mmol) in 2-propanol/water (2:1, 200 mL) was purged with N2 for 5 minutes. To this mixture was added [1,1′-bis(diphenyl-phosphino)ferrocene]dichloropalladium(II) (816 mg, 1.09 mmol) and the mixture was heated at reflux for 20 h. The mixture was allowed to cool to ambient then diluted with water (400 mL) and extracted with EtOAc (2×300 mL). The combined organic extracts were washed with 1M aqueous HCl, brine, dried (MgSO4), filtered through a plug of Celite and the filtrate reduced in vacuo to give the title compound (11.1 g) as a brown gum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08530469B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-bf2af01711cc46c7809154f7274604a4 |
| Source note | uspto-grants-2013_09 |