HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(2,6-Dichloro-3,5-dimethoxy-phenyl)-3-[6-(4-dimethylaminomethyl-2-nitro phenylamino)-pyrimidin-4-yl]-3-methyl-1-(2-trimethylsilanyl-ethoxymethyl)-urea → 1-[6-(2-Amino-4-dimethylaminomethyl-phenylamino)-pyrimidin-4-yl]-3-(2,6-dichloro-3,5-dimethoxy-phenyl)-1-methyl-3-(2-trimethylsilanyl-ethoxymethyl)-urea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(2,6-Dichloro-3,5-dimethoxy-phenyl)-3-[6-(4-dimethylaminomethyl-2-nitro phenylamino)-pyrimidin-4-yl]-3-methyl-1-(2-trimethylsilanyl-ethoxymethyl)-urea | HCID 131736972 | — |
| Catalyst | Chlorobenzene | HCID 7964 | — |
| Catalyst | Adams' catalyst | HCID 345198 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-[6-(2-Amino-4-dimethylaminomethyl-phenylamino)-pyrimidin-4-yl]-3-(2,6-dichloro-3,5-dimethoxy-phenyl)-1-methyl-3-(2-trimethylsilanyl-ethoxymethyl)-urea | HCID 131736973 | — |
Reaction Steps
To a stirred solution of 1-(2,6-dichloro-3,5-dimethoxy-phenyl)-3-[6-(4-dimethylaminomethyl-2-nitro-phenylamino)-pyrimidin-4-yl]-3-methyl-1-(2-trimethylsilanyl-ethoxymethyl)-urea (100 g, 0.15 mmol) in MeOH (10 mL) was added 4 drops of chlorobenzene and then PtO2 (30 mg, 30% wt). The solution was stirred under hydrogen atmosphere at room temperature overnight. The reaction was filtered and concentrated. The residue was taken to the next step without further purification. MS (ESI): 650 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434697B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-e3aa4daf10934ef5b60e03ae04bab335 |
| Source note | uspto-grants-2016_09 |