HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-butyl N-((3-(aminomethyl)phenyl)methyl)carbamate → {3-[(5-Nitro-4-thiocyanato-pyrimidin-2-ylamino)-methyl]-benzyl}-carbamic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-butyl N-((3-(aminomethyl)phenyl)methyl)carbamate | HCID 2756043 | — |
| Reactant | 2-Chloro-5-nitropyrimidin-4-yl thiocyanate | HCID 21077588 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | {3-[(5-Nitro-4-thiocyanato-pyrimidin-2-ylamino)-methyl]-benzyl}-carbamic acid tert-butyl ester | HCID 57885599 | 56.8% |
Reaction Steps
To a solution of 2-chloro-5-nitro-4-thiocyanato-pyrimidine (1.31 g, 6.05 mmol) in EtOH (10 mL) at 0° C. was added a solution of (3-aminomethyl-benzyl)-carbamic acid tert-butyl ester (1.43 g, 6.05 mmol) dropwise over 45 min. The reaction was allowed to stir at room temperature overnight and the resulting precipitate filtered and washed with EtOH. The crude material was purified by column chromatography (silica gel, 10:90 to 12:88 EtOAc/hexane) to afford {3-[(5-nitro-4-thiocyanato-pyrimidin-2-ylamino)-methyl]-benzyl}-carbamic acid tert-butyl ester (1.43 g, 56%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601714B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-e9f09ac04c6149379f9f06c532788f9d |
| Source note | uspto-grants-2009_10 |