関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4,6-Trimethylaniline | HCID 6913 | — |
| 反応物 | 2,4,5,6-Tetrachloropyrimidine | HCID 15690 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2,5,6-trichloro-N-(2,4,6-trimethylphenyl)4-pyrimidinamine | HCID 22170091 | — |
| 生成物 | 4,5,6-trichloro-N-(2,4,6-trimethylphenyl)-2-pyrimidinamine | HCID 22170094 | — |
反応手順
2,4,5,6-tetrachloropyrimidine (0.0134 mol), 1,4-dioxane (30 ml), 2,4,6-trimethyl aniline (0.0134 mol), and N,N-bis(1-methylethyl)ethanamine (0.0136 mol) were added to a flask under argon and stirred at 55° C. for 16 hours. The solvent was evaporated, and the residue was dissolved in CH2Cl2, then purified by column chromatography over silica gel (eluent: CH2Cl2/hexane ¼, and ½). The desired fractions were collected and their solvent was evaporated, yielding 0.15 g 4,5,6-trichloro-N-(2,4,6-trimethylphenyl)-2-pyrimidinamine (interm. 6) and 3.15 g 2,5,6-trichloro-N-(2,4,6-trimethylphenyl)-4-pyrimidinamine (interm. 7).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530655B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-489dd9ecf56a4150bd590657d4a5ef5d |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
