Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 10090741 | HCID 10090741 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19012158 | HCID 19012158 | — |
Reaction Steps
15 ml of a chloroform solution containing 1.0 g of 6-[4-(3-[4-aminophenoxy]propyl)piperazin-1-yl]-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione obtained in Example 6 and 2.5 ml of triethylamine was added to 5 ml of a chloroform solution containing 1.5 g of methanesulfonyl chloride, and the solution was then stirred at room temperature for 30 minutes. Afterward, water was added to the solution, and this solution was then subjected to separation, drying, concentration and purification through a silica gel column chromatograph (chloroform/methanol=50/1). Next, the thus obtained 1,3-dimethyl-6-[4-(3-[4-dimethanesulfonylaminophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione was treated with an HCl/methanol solution in an ordinary manner to obtain 0.75 g of crystalline 1,3-dimethyl-6-[4-(3-[4-dimethanesulfonylaminophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.hydrochloride (Compound 83).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05332739 |
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| Source dataset | uspto-grants-1994_07 |
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| ORD ID | ord-72540d647e7f4253ac41f87040bd2c4f |
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| Source note | uspto-grants-1994_07 |
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