HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 131733362, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 1-Chloro-N,N-2-trimethylpropenylamine | HCID 640792 | — |
| Reactant | HCID 117831217 | HCID 117831217 | — |
| Reactant | HCID 131733363 | HCID 131733363 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 131733362 | HCID 131733362 | — |
Reaction Steps
The acid obtained in Step B (9 g, 11.8 mmol) is dissolved in 90 mL of 1,2-dichloroethane. 1.9 mL of 1-chloro-N,N,2-trimethylpropenylamine (14 mmol) are added thereto. After stirring for 3 hours at ambient temperature, 90 mL of toluene and 4.62 g of N-[4-[tert-butyl(dimethyl)silyl]oxyphenyl]-1-methyl-1H-pyrrolo[2,3-b]pyridin-5-amine (Preparation 3″, 13 mmol) are added. The reaction mixture is heated at 110° C. for 20 hours. After returning to ambient temperature, the reaction mixture is washed with brine, dried over Na2SO4, filtered and concentrated to dryness. The residue obtained is purified by chromatography over silica gel (dichloromethane/ethanol gradient) to yield the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115159B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-aee84fecb90844aab953f240504a0b60 |
| Source note | uspto-grants-2015_08 |