HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 75232Generated: October 29, 2026
Triisopropyl phosphate → 2-[2,6-Dichloro-4-(ethylthio)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepine bis(trifluoroacetate)
https://huagongshe.com/reaction/75232
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triisopropyl phosphate | HCID 68188 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 2,6-Dichloro-4-(ethylthio)benzaldehyde | HCID 86613276 | — |
| Reactant | HCID 178525666 | HCID 178525666 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-[2,6-Dichloro-4-(ethylthio)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepine bis(trifluoroacetate) | HCID 86613277 | — |
Reaction Steps
A solution of (6Z)-5H-dipyrido[2,3-b:4′,3′-f]azepine-5,6(11H)-dione 6-oxime trifluoroacetate (200 mg, 0.4 mmol), 2,6-dichloro-4-(ethylthio)benzaldehyde (200 mg, 0.85 mmol) and ammonium acetate (0.60 g, 8.0 mmol) were stirred in acetic acid (3 mL) and heated in a microwave for 5 minutes at 130° C. Evaporation gave the crude product which was dissolved in acetonitrile (1.0 mL) and triisopropyl phosphate (100 μL, 0.4 mmol) and heated in a microwave for 5 minutes at 180° C. Purification by preparative LCMS gave the desired product LC/MS: 440 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08835423B2 |
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| Source dataset | uspto-grants-2014_09 |
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| ORD ID | ord-7a4d5407d9334c629fad306666b78b57 |
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| Source note | uspto-grants-2014_09 |
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