HuagongsheHuagongshe Chemistry Print Report · For research reference only
Calcium Chloride → HCID 22141140, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 22141298 | HCID 22141298 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22141140 | HCID 22141140 | 99% |
Reaction Steps
To a solution of 3-allyl-6-methyl-6-(3-nitrophenyl)-3-azabicyclo[3.1.0]hexan-2-one (Preparation 50, 10.2 g, 37.5 mmol) in ethanol (850 ml) and water (150 ml) was added iron powder (18.9 g, 337.5 mmol) and calcium chloride (2.1 g, 18.7 mmol). The reaction mixture was refluxed for 5 h, and then filtered to remove the iron powder. The reaction mixture was concentrated in vacuo and the residue was dissolved in dichloromethane:methanol (85:15), filtered and then concentrated in vacuo, dissolved in tetrahydrofuiran, filtered and then concentrated in vacuo to give the title compound as a pale yellow foam (9 g, 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313312B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-b9a59e2b720a47a9aa66a2ed6ddf2339 |
| Source note | uspto-grants-2001_11 |