HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → 5-Azaspiro[2.4]heptan-4-one, 7-amino-7-methyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Hexamethyldisilazane | HCID 13838 | — |
| Reactant | 1-(1,2-Diamino-1-methylethyl)-1-cyclopropanecarboxylate dihydrochloride | HCID 57434368 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 5-Azaspiro[2.4]heptan-4-one, 7-amino-7-methyl- | HCID 55282119 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To an acetonitrile solution (70 mL) of the crude product (800 mg, 3.46 mmol) of 1-(1,2-diamino-1-methylethyl)-1-cyclopropanecarboxylate dihydrochloride was added 1,1,1,3,3,3-hexamethyldisilazane (7.38 mL, 34.6 mmol), and the mixture was heated under reflux under a nitrogen atmosphere in an oil bath at 100° C. for 4 hours. Then the solution was cooled to room temperature, and to the solution was added methanol (70 mL). After that, the solvent was removed under reduced pressure. Thus a crude product of 7-amino-7-methyl-5-azaspiro[2.4]heptan-4-one was obtained as a light brown gum-like solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003666B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-3486e2102cc74134a5816f19c1149860 |
| Source note | uspto-grants-2011_08 |