HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-[2-[(2-Nitrophenyl)methyl]3-thienyl]-1,3-dioxolane → 4,10-Dihydro-5H-thieno[3,2-c][1]benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-[2-[(2-Nitrophenyl)methyl]3-thienyl]-1,3-dioxolane | HCID 11130065 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 4,10-Dihydro-5H-thieno[3,2-c][1]benzazepine | HCID 10867366 | 72.4% |
Reaction Steps
A stirred solution of 4 gms of 2-[2-[(2-nitrophenyl)methyl]-3-thienyl]-1,3-dioxolane in acetone (50 ml) and acetic acid (90% 50 ml) is heated to 60° C. Zinc dust (10 gms) is slowly added and after the addition, reaction mixture is stirred for 6 hours. At the end, reaction mixture is filtered and the residue washed with acetone and concentrated. The brown residue is extracted with chloroform and washed well with water. The organic layer is dried (Na2SO4) and filtered and concentrated. The product is isolated by silica gel column chromatography by eluting with 20% ethyl acetate:hexane to give 2.0 g of the desired product as a pale yellow crystalline solid, m.p. 86° C. Mass Spectrum; M+ 202.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05760031 |
| Source dataset | uspto-grants-1998_06 |
| ORD ID | ord-64e33ffc2ee6440bbb6bd37b6ea89420 |
| Source note | uspto-grants-1998_06 |