HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 58045794, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phenyltrimethylammonium bromide dibromide | HCID 17977687 | — |
| Reactant | HCID 58136802 | HCID 58136802 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 58045794 | HCID 58045794 | 116.5% |
Reaction Steps
1-{3-tert-Butyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]phenyl}ethanone (O2.059; 3.4 g) was dissolved in methanol/THF (50/50 ml) and admixed while stirring with phenyltrimethylammonium tribromide (4.21 g). After stirring at RT for 3 h, 20% citric acid solution was added and the mixture was stirred for 1 h. Then EA was added and the EA phase was removed. The EA phase was dried over magnesium sulfate and concentrated by rotary evaporation. The residue was purified by means of silica gel (80 g cartridge, n-heptane/EA gradient of 0-50% within 60 min). 2.49 g of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076336B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-3f798f37115f49b4bcf30832306d61dd |
| Source note | uspto-grants-2011_12 |