HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 7-Methoxy-1,2,3,4-tetrahydronaphthalen-1-one | HCID 81276 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one | HCID 676953 | 71.1% |
Reaction Steps
4 g of sodium azide are added portionwise to 8.3 g of 7-methoxy-1-tetralone in 36 ml of acetic acid. Then 17 ml of concentrated sulphuric acid are added dropwise, without a rise in temperature over 40°; the solution is poured onto ice and neutralised with 2 N sodium hydroxide solution. The separating bulk of crystals is removed and recrystallised from ethyl acetate. One obtains 6.4 g of 8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one (m.p. 137°-138°).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04322439 |
| Source dataset | uspto-grants-1982_03 |
| ORD ID | ord-4c47795adde74da0954b17145309aafe |
| Source note | uspto-grants-1982_03 |