HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibenzo[b,e]thiepin-11(6H)-one → Dibenzo[b,e]thiepin-11(6H)-one, oxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibenzo[b,e]thiepin-11(6H)-one | HCID 73741 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | Dibenzo[b,e]thiepin-11(6H)-one, oxime | HCID 73794634 | — |
Reaction Steps
19.7 G. of dibenzo[b,e]thiepin-11(6H)-one and 14.6 g. of hydroxylamine hydrochloride in 350 ml. of pyridine are stirred under reflux conditions for 16 hours. After the addition of a further 7.3 g. of hydroxylamine hydrochloride, the mixture is stirred for a further 5 hours under reflux conditions. The mixture is evaporated and purified by chromatography over aluminum oxide using chloroform and chloroform/methanol (93:3) for the elution. The purified product is recrystallized from acetone. There is obtained dibenzo[b,e]thiepin-11(6H)-one-oxime of melting point 241°-243° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03985895 |
| Source dataset | uspto-grants-1976_10 |
| ORD ID | ord-0b71075db16e47b086aeb1165e17c4f9 |
| Source note | uspto-grants-1976_10 |