HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 136082911, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridinium chloride | HCID 10176127 | — |
| Reactant | HCID 66749847 | HCID 66749847 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 136082911 | HCID 136082911 | 69% |
Reaction Conditions
| Temperature | 200 °C |
|---|
Reaction Steps
A mixture of 24.2 g (82.5 mmol) of 2-({6-methoxy}-1H-indazol-3-yl)-1H-isoindole-1,3(2H)-dione and 73.4 g (0.635 mol) of piridine hydrochloride was heated at 200° C. for 4 hours. The resulting brown solution was cooled to 140° C. and slowly poured in a well stirred mixture of 250 ml of 0.2 N HCl and 350 ml of ethyl acetate. The organic layer was separated and the aqueous layer was salted (45 g of NaCl) and extracted twice with 350 ml of ethyl acetate. Organic extracts were dried over sodium sulfate and concentrated under vacuum to small volume. The precipitate was filtered off and dried: 15.89 g of product as yellow solid were obtained. Yield=68.9%. mp=265-270° C. dec.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07511136B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-f12aead606f24a7b964da767f75a6aec |
| Source note | uspto-grants-2009_03 |