Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 10550087 | HCID 10550087 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19016828 | HCID 19016828 | 49.8% |
Reaction Steps
To a solution of 0.5 g of 9-acetyl-2-(4-chlorophenyl)-5,6-dihydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7,7-dioxide obtained in Example 48 in a mixed solvent of 40 ml of methanol and 30 ml of chloroform is added 0.1 g of sodium borohydride under ice-cooling and the mixture is stirred for 30 minutes at room temperature. After the completion of reaction, to the mixture is added water and the solution is extracted with chloroform. The extract is washed with water, dried and concentrated under reduced pressure. The resulting crystals are recrystallized with ethanol to give 0.25 g of 2-(4-chlorophenyl)-9-(1-hydroxyethyl)-5,6-dihydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7,7-dioxide as white crystals, melting at 233°-235° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05329016 |
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| Source dataset | uspto-grants-1994_07 |
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| ORD ID | ord-6b13c1f80a5b4ea3a5a81b833e594eb3 |
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| Source note | uspto-grants-1994_07 |
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