HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic anhydride → HCID 15817308, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 54162170 | HCID 54162170 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 15817308 | HCID 15817308 | 77% |
Reaction Steps
The acid from Step 5 (7.63 g, 33 mmol) was dissolved in trifluoroacetic acid (12 mL), treated with trifluoroacetic anhydride (4 mL) and stirred at room temperature (8 minutes). The reaction was poured into 10% Na2CO3 (50 mL) and extracted with ethyl acetate, washed with brine, dried over MgSO4 and concentrated in vacuo to give 8-fluoro-7-methoxyisothiochroman-4-one (5.42 g, 77%) as a brown solid: mp 85°-92° C.; 1H NMR (CDCl3) 300 MHz 7.83 (d, J=8.9 Hz, 1H) 7.19 (t, J=8.5 Hz, 1H) 4.01 (s, 2H) 3.98 (s, 3H) 3.55 (s, 2H); 19F NMR (CDCl3) 300 MHz -141.24 (m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05565482 |
| Source dataset | uspto-grants-1996_10 |
| ORD ID | ord-6c37d90c411e4f919600abb250afc4ca |
| Source note | uspto-grants-1996_10 |