HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 2-chloro-N-methyl-5-nitropyrimidin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4-Dichloro-5-nitropyrimidine | HCID 521266 | — |
| Reactant | Methylamine ethanol | HCID 22028356 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-chloro-N-methyl-5-nitropyrimidin-4-amine | HCID 7147232 | 85.4% |
Reaction Steps
A solution of methyl amine-ethanol (7.6 ml) and N,N-diisopropylethylamine (13.2 ml) were dissolved into 150 ml dichloromethane. The mixture was added dropwise to a solution of 2,4-dichloro-5-nitropyrimidine (10.0 g) in dichloromethane (30 ml) at 0° C. After the completion of the dropwise addition, the mixture was kept at the same temperature to react for half an hour. Purification was conducted by a column chromatography to obtain a yellow solid (8.3 g) in a yield of 85.4%. 1H NMR (400 MHz, CDCl3): δ 9.05 (s, 1H), 8.41 (s, 1H), 3.22 (s, 3H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096601B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-075d87a7989c43cca1cf80dc2d258182 |
| Source note | uspto-grants-2015_08 |