HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Aminoacetophenone → HCID 2994007, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Aminoacetophenone | HCID 7468 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 2994007 | HCID 2994007 | 97.9% |
Reaction Steps
To a stirred solution of 10 g of 4-aminoacetophenone (74 mmol, 1 eq) in a mixture of 60 ml of water and 100 ml of dioxane at 0° C., 12.43 g of NaHCO3 (148 mmol, 2 eq) and 15.3 g of benzyl chloroformate (85 mmol, 1.15 eq, purity 95%) are added. The mixture is stirred at room temperature for 4 h and then concentrated under reduced pressure to remove the dioxane. The suspension is diluted with 70 ml of water and 150 ml of ethyl acetate. The phases are separated and the organic layer is washed with 2×50 ml of brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give 19.5 g of the product as solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802858B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-05b81ddee8b547ff81a56de1f1d60c4a |
| Source note | uspto-grants-2014_08 |