関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4,6-Dichloro-2-methylpyrimidin-5-amine | HCID 736674 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 6-Chloro-2-methylpyrimidine-4,5-diamine | HCID 594145 | 91% |
反応手順
A 200 mL stainless steel Parr vessel was loaded with 5-amino-4,6-dichloro-2-methylpyrimidine (7.2 g, 40 mmol) and 2 M ammonia in isopropanol (100 mL), and then was sealed and heated at 150° C. for 16 h. HPLC analysis indicated complete conversion. The mixture was concentrated in vacuo, and the residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL). This was stirred at 50° C. for 1 h and then was cooled to room temperature. The precipitate was collected by suction filtration, washed sparingly with isopropanol, then air dried on the filter to afford 6-chloro-4,5-diamino-2-methylpyrimidine (5.8 g, 91%) as a brown powder, which was used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08895568B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-e243258ad81a4b0185dda7b3f4dc6261 |
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| 出典メモ | uspto-grants-2014_11 |
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