HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 67608694, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67606947 | HCID 67606947 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67608694 | HCID 67608694 | 55% |
Reaction Steps
A solution of carbamate 90 (175 mg, 0.29 mmol) in DCM (10 mL) was treated with TFA (4 mL) at 0° C. After 1.5 h, the reaction mixture was concentrated, diluted with EtOAc, washed successively with saturated aqueous NaHCO3, and brine dried over anhydrous Na2SO4, filtered and concentrated. The crude residue was purified by reverse phase HPLC (2″ Dynamax® C18; 10% ACN/water to 70% ACN/water containing 0.1% HOAc, 30 min; Flow: 40 mL/min). The product-containing fractions were combined, frozen, and lyophilized to afford 91 (80 mg, 55%) as a white flocculent solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415486B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-edc149cf4fd14cbd84cfbcb552ec36e5 |
| Source note | uspto-grants-2013_04 |