HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 53781817, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium amide | HCID 24533 | — |
| Reactant | HCID 54433857 | HCID 54433857 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Hexamethylphosphoramide | HCID 12679 | — |
| Product | HCID 53781817 | HCID 53781817 | — |
Reaction Steps
4-Methyl-6-phenyl-1-oxa-3-azaspiro [4.5] decan-2-one (Example XXIII) (23.6 g) in hexamethylphosphoric triamide (HMPT) is added dropwise to 5 g sodium amide in 35 ml HMPT. The mixture is stirred until NH3 evolution is essentially finished and 11 ml methyl iodide added at about 40° over a 1/2 hour period. The mixture is stirred 1 hour, added to 700 ml water and extracted with ethyl acetate. The extract is washed with water, dried and concentrated to give 25 g crude product. A sample of the crude product, recrystallized from cyclohexane, gave the crystalline product, m. 85°-6°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03974157 |
| Source dataset | uspto-grants-1976_08 |
| ORD ID | ord-f8d479b70e0c47d9a38a615a8e762565 |
| Source note | uspto-grants-1976_08 |