HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23353984, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 23354006 | HCID 23354006 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 23353984 | HCID 23353984 | 71% |
Reaction Steps
To a suspension of 1.4 g of 9-formyl-2-(4-methylphenyl)-2,5,6,7-tetrahydro-3H-thieno-[2',3':6,7]cyclohepta[1,2-c]pyridazin-3-one in methanol was added 1.0 g of sodium borohydride under ice-cooling. After stirring for an hour, the mixture was poured into diluted hydrochloric acid and extracted with chloroform. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a silica gel column using chloroform as an eluent. The solid was recrystallized from a mixed solvent of ethanol and isopropyl ether to give 1.0 g of 9-hydroxymethyl-2-(4-methylphenyl)-2,5,6,7-tetrahydro-3H-thieno-[2',3':6,7]cyclohepta[1,2-c]pyridazin-3-one as a white powder, melting at 158°-159° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05597918 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-73584c2e2d4a4c8da13ec1c15e6b7d61 |
| Source note | uspto-grants-1997_01 |