HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → N-(1,4-dioxaspiro[4.5]dec-8-yl)-1H-pyrazol-5-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 178418806 | HCID 178418806 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | N-(1,4-dioxaspiro[4.5]dec-8-yl)-1H-pyrazol-5-amine | HCID 67009993 | 64% |
Reaction Steps
A solution of 1H-pyrazol-3-amine (10.0 g) and 1,4-dioxaspiro[4.5]decan-8-one (20.7 g) in methanol (30 mL) was stirred at room temperature for 30 min. After stirring, a solution of sodium tetrahydroborate (3.6 g) in 1 M sodium hydroxide (30 mL) was added dropwise at 0° C. After warming to room temperature, the mixture was stirred for 4 hr, 1 M hydrochloric acid (100 mL) was added dropwise at 0° C., and the mixture was stirred for 1 hr. The resulting solid was collected by filtration, washed with water, and dried by heating under reduced pressure to give the title compound as a pale-yellow solid (17.2 g, 64%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592431B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-19c5a328d0744f388f789af34f39db77 |
| Source note | uspto-grants-2013_11 |