関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Boron Trichloride | HCID 25135 | — |
| 反応物 | HCID 178508616 | HCID 178508616 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178508615 | HCID 178508615 | 96.1% |
反応手順
A solution of trans 1-{3-[(benzyloxy)methyl]cyclobutyl}-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (0.244 g, 0.00051 mol) in dichloromethane (10 mL) was cooled to −78° C. and a solution of 1.0 M boron trichloride in dichloromethane (1.53 mL, 0.00153 mol) was added dropwise, keeping the temperature less than −70° C. The reaction mixture was stirred seven hours at −78° C., after which time a 8 M solution of ammonia in methanol (1.5 mL) was added . The solvent was removed in vacuo. The residue was purified by flash column chromatography on silica using dichloromethane/methanol (93:7). The solvent was removed in vacuo to give to give trans 3-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]cyclobutylmethanol (0.192 g, 0.00049 mol) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06660744B1 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-33b50eac03e842e69f9881339961918f |
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| 出典メモ | uspto-grants-2003_12 |
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