HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 67325553, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 67325480 | HCID 67325480 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67325553 | HCID 67325553 | 289.3% |
Reaction Steps
To a suspension of 3.56 g (54.49 mmol) of zinc powder in 15 mL of concentrated aqueous 33% NH4OH solution are added 1.2 g (5.45 mmol) of the product prepared in step 9.1 dissolved in 15 mL of tetrahydrofuran. The mixture is stirred for 1 hour at room temperature, the zinc is then separated out by filtration and the mixture is extracted with ether. The organic phases are combined, dried over Na2SO4, filtered and concentrated under vacuum. The oily residue is purified by chromatography on a column of silica, eluting with a cyclohexane/ethyl acetate gradient (70/30 to 60/40). 3 g of the expected product are obtained in the form of a yellow oil. Quantitative yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975250B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-6eded6adab5c43ccb5e7b29d20671839 |
| Source note | uspto-grants-2015_03 |