HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tin atom → HCID 20027814, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tin atom | HCID 5352426 | — |
| Reactant | 1-(4-Nitrophenyl)-3-propargyl-3-azabicyclo[3.1.1]heptane-2,4-dione | HCID 20027832 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20027814 | HCID 20027814 | — |
Reaction Steps
A mixture of 1.6 g of 1-(4-nitrophenyl)-3-propargyl-3-azabicyclo[3.1.1]heptane-2,4-dione and 4.2 g of tin powder in 12 ml of water and 12 ml of concentrated hydrochloric acid is stirred at 100° for 1 hour. After cooling to room temperature, the reaction mixture is diluted with a little water, filtered and rendered alkaline by the addition of sodium hydroxide solution. The reaction mixture is extracted with ethyl acetate, and the organic phase is washed neutral with dilute sodium chloride solution, dried over magnesium sulphate and concentrated by evaporation. After purification by chromatography over silica gel in the system ethyl acetate/hexane 1:1, the title compound is obtained. Rf (ethyl acetate/hexane 1:1)=0.15.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04677129 |
| Source dataset | uspto-grants-1987_06 |
| ORD ID | ord-7319a70db20743449e2a11335b274989 |
| Source note | uspto-grants-1987_06 |