HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 70207479, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 70204323 | HCID 70204323 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 70207479 | HCID 70207479 | 90.3% |
Reaction Steps
In 150 ml of methanol, is dissolved 9.33 g (21.6 mmol) of trans-1-benzyloxycarbonyl-3-phthalimidomethyl-4-trifluoromethylpyrrolidine. To the above solution, is added 2.1 ml (43.2 mmol) of hydrazine monohydrate, and the mixture is stirred at room temperature for 12 hours. The resulting precipitate is removed by filtration, and the filtrate is concentrated under reduced pressure. The residue is dissolved in dichloromethane and washed with water. The washed solution is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (elusion solvent; chloroform/methanol (100/2→100/5)) to give 5.89 g of the objective substance as a yellow oily matter (yield 90.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05668147 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-3affa2a7b07648cd801e5b8199671911 |
| Source note | uspto-grants-1997_09 |