HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → Trifluoroacetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 9-[8-(2,2,2-Trifluoro-acetyl)-8-aza-bicyclo[3.2.1]oct-3-ylidene]-9H-xanthene-3-carbonitrile | HCID 57725339 | — |
| Reactant | Acetic hydrazide benzenesulfonic acid | HCID 86636508 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 178433930 | HCID 178433930 | — |
Reaction Steps
A mixture of compounds 11a (0.029 g, 0.125 mmol) and 5e (0.051g, 0.124 mmol) was exposed to microwave irradition (300 W) at 200° C. for 10 min. After cooling, MeOH (1 mL) and 1N NaOH (1 mL) were added to the reaction mixture and the mixture was stirred at rt for 30 min. The crude product was purified by reverse phase HPLC to yield compound 35 as a TFA salt. MS m/z (MH+) 371.0; 1H NMR (CH3OH-d4) δ 1.40 (d, 2H), 1.85 (m, 2H), 1.41 (s, 3H), 3.02 (m, 4H), 3.91 (m, 2H), 7.19 (m, 4H), 7.33 (d, 2H), 7.84 (d, 1H), 7.85 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07553850B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-5844e01bb1154569be53d9dc0c6ea90d |
| Source note | uspto-grants-2009_06 |