HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 67460000, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | ethyl 3,5-dichloro-1H-pyrazole-1-acetate | HCID 67463975 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67460000 | HCID 67460000 | 32.7% |
Reaction Steps
A solution of ethyl 3,5-dichloro-1H-pyrazole-1-acetate (1.29 g, 5.8 mmol) (i.e. the product of Example 12, Step E) in tetrahydrofuran (10 mL) was treated with sodium hydroxide (5 mL, 15% aqueous solution) in water (3 mL), and the reaction mixture was stirred at ambient temperature for 1.5 h. The reaction mixture was then diluted with water (15 mL) and was concentrated under reduced pressure. The aqueous solution was acidified with concentrated hydrochloric acid to pH 1. The reaction mixture was then extracted with ethyl acetate and the extract was dried over MgSO4. The extract was then concentrated and recrystallized from 20% ethyl acetate in hexanes to give 370 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08586611B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-7730a7680d4b42e5bd0a849b9ce217ac |
| Source note | uspto-grants-2013_11 |