HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 67236248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 67235338 | HCID 67235338 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67236248 | HCID 67236248 | — |
Reaction Steps
To the mixture of the crude diethyl 1-{3-[(tert-butoxycarbonyl)amino-]-3-methylbutyl}-1H-indole-2,6-dicarboxylate from the preceding step in CH2Cl2 (3 mL) is added TFA (1.5 mL). The mixture is stirred at room temperature for 2 h. The solvent is evaporated and the residue dried in vacuo. To a solution of the residue in ethanol (8 mL). is added triethylamine (0.13 mL, 0.90 mmol) and K2CO3 (124 mg, 0.90 mmol). The mixture is heated at 80° C. for 2 h and at 100° C. for 64 h. Water (20 mL) and acetic acid (1 mL) are added and the mixture is extracted with EtOAc. The organic layers are dried (Na2SO2) and concentrated to afford the title compound which is used in the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150577B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-80ae1f95fd2e491ab719a72a52e359d0 |
| Source note | uspto-grants-2015_10 |