HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 67619373, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 67619063 | HCID 67619063 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67619373 | HCID 67619373 | 86.3% |
Reaction Steps
To 200 mg (0.68 mmol) of cis-3-amino-4-methyl-1-(1-methylindazol-3-ylcarbonyl)pyrrolidine hydrochloride was added 0.7 ml of pyridine, and 0.07 ml (0.75 mmol) of acetic anhydride was added dropwise under ice cooling. Then, after heated to room temperature, the mixture was stirred overnight. To the reaction mixture was added water, and then the solution was extracted with methylene chloride. After washed with saturated saline solution and dried over anhydrous magnesium sulfate, the solution was concentrated under reduced pressure to obtain crude oil. This was subjected to silica gel column chromatographic purification (methylene chloride:acetone=10:1) to obtain 176 mg (86.3%) of aimed compound. m.p. 202°-204° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05449787 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-af5149e5e45a4c3e8368f808f65c084c |
| Source note | uspto-grants-1995_09 |