HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66887168, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | [3,5-Dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepin-2-yl)phenyl]methanol bis(trifluoroacetate) | HCID 86613275 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 66887168 | HCID 66887168 | 67.6% |
Reaction Steps
To a solution of [3,5-dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4′,3′-f]azepin-2-yl)phenyl]methanol bis(trifluoroacetate) (20.0 g, 0.03 mmol) in toluene (1.0 mL) was added triethylamine (11 μL, 0.08 mmol) and stirred for 5 minutes, followed by the addition of thionyl chloride (5.0 μL, 0.06 mmol) at room temperature for 16 hours. The reaction mixture was diluted with methanol and purified by preparative LCMS at pH 10 to give the desired product (8.7 mg, 65%). LC/MS: 428 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835423B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-3af09b28b43f4b38ae7f135d9f2473e9 |
| Source note | uspto-grants-2014_09 |