Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 67316730 | HCID 67316730 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67315421 | HCID 67315421 | — |
Reaction Steps
To a cooled (0° C.) solution of EXAMPLE 168A (880 mg) in tetrahydrofuran (10 mL) and dichloromethane (2 ml) and triethylamine (2 ml) was added, followed by the addition of trifluoroacetic anhydride (2 ml) dropwise. After the addition, the mixture was stirred for 3 hours at 0° C. After this time the mixture was diluted with ethyl acetate (200 mL) and water (80 mL). The aqueous layer was extracted with ether twice. The combined extracts were washed with water (×3), brine and dried over Na2SO4. Evaporation of solvent gave crude product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08853209B2 |
|---|
| Source dataset | uspto-grants-2014_10 |
|---|
| ORD ID | ord-bdeeefcffdac494a9c00ae7da5ba7956 |
|---|
| Source note | uspto-grants-2014_10 |
|---|