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2-Chloropyrimidine → HCID 19785323、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloropyrimidine | HCID 74404 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-[1-(2-aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine | HCID 19785318 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 19785323 | HCID 19785323 | 67% |
反応手順
A mixture of 1.7 parts of 2-chloropyrimidine, 5.5 parts of N-[1-(2 aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine, 1.5 parts of sodium hydrogen carbonate and 160 parts of ethanol was stirred and refluxed for 20 hours. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile, yielding 4.5 parts (67%) of 9-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyrimidinylamino)ethyl]-4-piperidinyl]-9H-purin-8-amine; mp. 164.1° C. (compound 164).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258380 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-547c46afb598489a92369f1f60ef5336 |
| 出典メモ | uspto-grants-1993_11 |