HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 86735559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86735560 | HCID 86735560 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 86735559 | HCID 86735559 | 61% |
Reaction Steps
A solution of 5.7 g. (0.030 moles) of cis-4,5-dimethyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one, 9 ml. (0.09 moles) of 35% aqueous formaldehyde solution and 0.05 g. of sodium hydroxide in 50 ml. of 92% ethanol is heated for 5 hours at 80° C., while stirring. The reaction mixture is cooled and the solvents are evaporated off in vacuo. The oil obtained is taken up in chloroform, washed several times with water and then dried over anhydrous sodium sulfate. After evaporation of the solvent in vacuo, the residual syrup is purified by recrystallization from diisopropyl ether. 4 g. (61% of theory) of cis-4,5-dimethyl-2-hydroxymethyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one are obtained. M.P. 91°-92° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04080449 |
| Source dataset | uspto-grants-1978_03 |
| ORD ID | ord-0b6c37427700447d9297eeca72791eff |
| Source note | uspto-grants-1978_03 |