HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 54427620, compound → HCID 19043379, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 54427620 | HCID 54427620 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19043379 | HCID 19043379 | 60.4% |
Reaction Steps
A solution of the intermediate 2 (5.8 g) in glacial acetic acid (50 ml) was added, dropwise, to a suspension of zinc dust (6.37 g) in glacial acetic acid (20 ml) cooled to 0°. The mixture was stirred at 23° for 3 h, then diluted with water (200 ml) and decanted from zinc. Solid sodium carbonate was added until pH=9 and the mixture extracted with ethyl acetate (2×300 ml). The combined organic extracts were washed with brine (300 ml), dried and concentrated in vacuo to an oil which was purified by flash chromatography (eluting in gradient from CH-EA 2:1 to EA) to give the title compound as a white foam (2.8 g). M.p. 125°-6°. T.l.c. DCM-methanol (30:1), Rf 0.38.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05580895 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-e1ac0e75c42e4de7b87425101b6f3c9b |
| Source note | uspto-grants-1996_12 |