HuagongsheHuagongshe Chemistry Print Report · For research reference only
trans-1,2-Diacetoxy-1,2-dihydrobenzocyclobutene → Rac-3',6',11'-triacetoxy-3'-acetyl-1',2',3',4',5',5a',6',11',11a',12'-decahydro-5',12'-dioxospiro[1,3-dithiolane-2,1'-naphthacene]
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | trans-1,2-Diacetoxy-1,2-dihydrobenzocyclobutene | HCID 13264175 | — |
| Reactant | Rac-3'-acetoxy-3'-acetyl-1',2',3',4',5',8'-hexahydro-5',8'-dioxospiro[1,3-dithiolane-2,1'-naphthalene] | HCID 20283284 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | Rac-3',6',11'-triacetoxy-3'-acetyl-1',2',3',4',5',5a',6',11',11a',12'-decahydro-5',12'-dioxospiro[1,3-dithiolane-2,1'-naphthacene] | HCID 20283287 | 79% |
Reaction Steps
A solution of 220 mg (1.0 mmol) of trans-1,2-diacetoxy-1,2-dihydrobenzocyclobutene and 234 mg (0.66 mmol) of rac-3'-acetoxy-3'-acetyl-1',2',3',4',5',8'-hexahydro-5',8'-dioxospiro[1,3-dithiolane-2,1'-naphthalene] [prepared as described in Example 5(A)] in 15 ml of dry xylene was stirred and heated under reflux under an atmosphere of nitrogen for 30 minutes. The pale orange solution was evaporated and the resulting yellow oil was triturated with 15 ml of diethyl ether to yield 298 mg (79%) of rac-3',6',11'-triacetoxy-3'-acetyl-1',2',3',4',5',5a',6',11',11a',12'-decahydro-5',12'-dioxospiro[1,3-dithiolane-2,1'-naphthacene] in the form of a pale yellow solid of melting point 135°-145° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04409391 |
| Source dataset | uspto-grants-1983_10 |
| ORD ID | ord-d13c1aceeb604cfb8aa03fd5b3672ca2 |
| Source note | uspto-grants-1983_10 |