Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 135710757 | HCID 135710757 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 135710756 | HCID 135710756 | 68.9% |
Reaction Steps
0.21 g of 3-methyl-5-(2-chlorophenyl)-8-(3-butynyloxycarbonyl)-6,7,8,9-tetrahydro-1H,3H-pyrido[4',3':4,5]thieno[3,2-f][1,4]diazepin-2-one was dissolved in 10 ml of dimethoxyethane, to which 0.11 g of sodium hydrogencarbonate and 0.22 g of phosphorus pentasulfide was added, followed by heating at 80° C. for 3 hours. After completion of the reaction, dichloromethane and methanol were added, and the mixture was filtered, followed by addition of silica gel to the resultant filtrate and evaporating the solvent to dryness. Silica gel column chromatography (elution solvent: dichloromethane:methanol=99:1) was used for purification, thereby obtaining 0.15 g of the intended compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05382579 |
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| Source dataset | uspto-grants-1995_01 |
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| ORD ID | ord-7e8935cded724801b9c0298481e02dab |
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| Source note | uspto-grants-1995_01 |
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