HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 13446113, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 3-(Methylamino)-1-benzoxepin-5(2H)-one | HCID 13446047 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 13446113 | HCID 13446113 | — |
Reaction Steps
Sodium borohydride is added in small portions to a solution of 18.8 g (0.1 mole) 3-methylamino-1-benzoxepin-5-(2H)-one in a mixture of 125 ml dioxane and 125 ml acetic acid cooled in an ice bath. The reaction solution is maintained in a cooled state during the addition of the sodium borohydride (0.4 mole) up to the end of the reaction. The reaction solution is then poured into ice water, made alkaline with sodium carbonate and extracted with dichloromethane. The organic solution is washed with saturated salt solution and dried over sodium sulfate. After removal of the solvent, 16.4 g (85% of the theoretical yield) of racemic-2,3,4,5-tetrahydro-3-methylamino-1-benzoxepin-5-ol is recovered in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04279904 |
| Source dataset | uspto-grants-1981_07 |
| ORD ID | ord-31c7455639ee4d86a48beee68e931064 |
| Source note | uspto-grants-1981_07 |