HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118045394, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 118046609 | HCID 118046609 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 118045394 | HCID 118045394 | 79.6% |
Reaction Steps
To 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazin-2-amine (8.68 g, 45.4 mmol) was added acetonitrile (368 mL), water (245 mL) and 3M HCl (76 mL). The reaction was stirred at room temperature for 30 min. The reaction was basified with excess 1M NaOH, and then diluted with of ethyl acetate. The organic layer was separated. The aqueous layer was extracted well with EtOAc/2-methyl THF (1:1) three times. Organic layers were combined and dried over Na2SO4, filtered and concentrated to give 6.91 g of product as free base. LCMS (m/z): 192.12 (MH+), 0.30 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242996B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-d8bd1161d774412ca00940241026c390 |
| Source note | uspto-grants-2016_01 |