HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 3-Chloro-2-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-4,5,6,7-tetrahydro-2H-indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one | HCID 19933459 | — |
| Product | 3-Chloro-2-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-4,5,6,7-tetrahydro-2H-indazole | HCID 19933460 | — |
Reaction Steps
0.2 g 2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one was treated with 2 ml phosphorus oxychloride and the mixture stirred for one hour under reflux. After cooling, it was poured into ice-water, extracted with ethyl acetate and the organic phase washed with sodium hydrogen carbonate and water. It was dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 0.07 g=32% of theory m.p.: 161°-163° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05424443 |
| Source dataset | uspto-grants-1995_06 |
| ORD ID | ord-ecab1ddb575c4a79813f70eaa9956a8a |
| Source note | uspto-grants-1995_06 |