HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 59591077, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 59591078 | HCID 59591078 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59591077 | HCID 59591077 | 211.8% |
Reaction Steps
Trifluoroacetic acid (20.0 ml) was added dropwise to a solution of butyl(2E)-3-[2-[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)ethyl]-3-methyl-4-(methyloxy)phenyl]-2-propenoate (Preparation 13; 950 mg, 2.43 mmol) in dichloromethane (20 ml) at 0° C. After 1 h at 0° C., the solvent was removed; purification using a sulphonic acid ion exchange cartridge (SCX; 20 g), eluting with dichloromethane followed by 2N ammonia in methanol, and evaporation of the methanol/ammonia phase gave a brown solid (1.5 g). The solid was triturated with toluene, the mixture filtered, and the mother liquor concentrated in vacuo and dried under vacuum to give the title compound as a brown oil (960 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08263620B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-b1e561278f6141b18c03b5e3cad91145 |
| Source note | uspto-grants-2012_09 |