Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Hexahydro-1,4-diazepine | HCID 68163 | — |
| Reactant | HCID 11063100 | HCID 11063100 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 10198826 | HCID 10198826 | 75.9% |
Reaction Steps
A 100 ml 3-necked flask equipped with a condenser, addition funnel and magnetic stirring bar and under a nitrogen atmosphere was charged with a solution of homopiperazine (3.0 g; 30.5 mmol) in DMAC (35 ml). Potassium iodide (300 mg) was added followed by the addition of a solution of 4-chloro-3,4-dihydro-2H-benzothiopyran (1.15 g; 6.1 mmol) in DMAC (15 ml). This solution was then heated in an oil bath at 60° C. overnight. The reaction mixture was partitioned between water and ethyl acetate, washed with brine and dried with magnesium sulphate. Filtration and evaporation of solvent gave a yellow oil (1.15 g) which exhibited a satisfactory proton nmr spectrum (300 MHz, CDCl3). This material was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06407093B1 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-476cd91aced844b181274070ed138c38 |
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| Source note | uspto-grants-2002_06 |
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