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Methylamine → 6-chloro-N-methylpyrimidin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4,6-Dichloropyrimidine | HCID 70943 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 6-chloro-N-methylpyrimidin-4-amine | HCID 309479 | 62% |
反応手順
To a solution of 4,6-dichloro-pyrimidine (7.45 g, 50 mmol) in iPrOH (50 mL) was added a solution of methyl amine in THF (2M, 30 mL, 60 mmol) at room temperature. The resulting mixture was stirred for 18 hours. The mixture was concentrated and the residue was purified by flash chromatography on silica eluting with DCM:EtOAc=6:1-1:1 to obtain the title compound (4.4 g, yield: 62%) as a white solid. 1H NMR (400 MHz, CDCl3) δ 2.96 (d, 3H), 5.22-5.36 (bs, 1H), 6.35 (s, 1H), 8.35 (s, 11H); MS (ESI): 144 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434697B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-be2f740bdb93431cbfa5a50b841b792a |
| 出典メモ | uspto-grants-2016_09 |