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5-Amino-4,6-dichloropyrimidine → 6-Chloro-N4-[1-(3,5-diisopropoxy-benzyl)-piperidin-4-yl]-pyrimidine-4,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| 反応物 | 1-(3,5-Diisopropoxy-benzyl)-piperidin-4-ylamine | HCID 59210370 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Diisopropylethylamine | HCID 81531 | — |
| 生成物 | 6-Chloro-N4-[1-(3,5-diisopropoxy-benzyl)-piperidin-4-yl]-pyrimidine-4,5-diamine | HCID 86618537 | 20% |
反応手順
A solution of 4,6-dichloro-pyrimidin-5-ylamine (19.7 mg, 0.12 mmol, 1.0 equiv; commercially available) and 1-(3,5-diisopropoxy-benzyl)-piperidin-4-ylamine (46.0 mg, 0.15 mmol, 1.25 equiv; intermediate A3) in N-ethyl diisopropylamine (1.0 mL) and acetonitril (1.0 mL) was heated by microwave irradiation to 160° C. for 20 min. Removal of the solvent under reduced pressure and purification by preparative HPLC on reversed phase eluting with a gradient of acetonitrile/water provided 10.6 mg (20%) of the title compound. MS (ISP): 434.3 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07968568B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-49a1894631f44386924bbbfc2a93bacc |
| 出典メモ | uspto-grants-2011_06 |