HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 20344037, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 20344062 | HCID 20344062 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 20344037 | HCID 20344037 | — |
Reaction Steps
A solution of 2.4 g of 10,11-dihydro-11-oxospiro[dibenz(b,f)thiepin-10,4'-piperidine], free base of Example 3, in 20 ml of tetrahydrofuran is added dropwise to a refluxing slurry of 1.5 g of lithium aluminum hydride in 20 ml of tetrahydrofuran. After total addition, stirring is continued at reflux for an addition 4 hours and then at ambient temperature for 16 hours. Thereafter, the reaction mixture is decomposed by adding sequentially 1.7 ml of water with 1.7 ml of 15% sodium hydroxide and 5.2 ml of water. The diluted mixture is filtered and the filtrate is concentrated under vacuum, providing 10,11-dihydro-11-hydroxyspiro[dibenz(b,f)thiepin-10,4'-piperidine].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04198420 |
| Source dataset | uspto-grants-1980_04 |
| ORD ID | ord-9e3ce6ee9dc843029edeed731712c6e0 |
| Source note | uspto-grants-1980_04 |