Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | 1-(2-Methoxyphenyl)piperazine | HCID 1346 | — |
| Reactant | HCID 14669080 | HCID 14669080 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 14797399 | HCID 14797399 | — |
Reaction Steps
To 150 ml of p-dioxane were added 11-(2-propynyl)-10,11-dihydro-5-methyl-5H-pyrido[3,4-f]pyrrolo[1,2-b][1,2,5]triazepine (2.3 g), 4-(2-methoxyphenyl)piperazine (2.1 g), paraformaldehyde (2.0 g), and CuCl (0.02 g). After stirring at 80° C. for three hours, the mixture was concentrated to 6.9 g of brown oil, which was eluted on a silica gel column with 5% methanol/DCM via HPLC. The desired fraction was concentrated to 4.3 g of 11-[1-[4-(2-methoxyphenyl)piperazin-1-yl]-2-butynyl]-10,11-dihydro-5-methyl-5H-pyrido[3,4-f]pyrrolo[1,2-b][1,2,5]triazepine, as a light brown oil; MS(EI)M+ @ 442 (6.7%), IR(CHCl3)--C≡CH @ 3300 cm-1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04996205 |
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| Source dataset | uspto-grants-1991_02 |
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| ORD ID | ord-2782063c843445abbecd324032c4258a |
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| Source note | uspto-grants-1991_02 |
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