HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic anhydride → Ethyl 7-oxo-1,4,5,6-tetrahydroindole-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | 4-(5-(Ethoxycarbonyl)-1H-pyrrol-3-yl)butanoic acid | HCID 15272822 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | Ethyl 7-oxo-1,4,5,6-tetrahydroindole-2-carboxylate | HCID 848532 | 87% |
Reaction Steps
Into a 1000-mL round-bottom flask was placed a solution of 113h (30 g, 133.19 mmol, 1.00 equiv) in CF3COOH (500 mL) and trifluoroacetyl 2,2,2-trifluoroacetate (42 g, 199.97 mmol, 1.50 equiv). See FIG. 14. The resulting solution was stirred at room temperature for 60 min, concentrated under vacuum, diluted with 500 mL of water and 500 mL of EA, and extracted with 3×500 mL of ethyl acetate. The combined organic layers were washed with 1×500 mL of saturated aqueous potassium carbonate and 1×500 mL of brine, dried over anhydrous sodium sulfate and concentrated under vacuum to afford 24 g (87%) of 113i as a light brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946213B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-911e7aa3be8246c69394e3531d8026a9 |
| Source note | uspto-grants-2015_02 |