関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4,5-Pyrimidinediamine, 6-chloro- | HCID 78010 | 71% |
反応手順
To a 7 N solution of ammonia in MeOH (40 mL) was added 4,6-dichloropyrimidin-5-ylamine (8.7 g, 53 mmol) and the solution was heated to 100° C. in a sealed tube. After 12 h, the resulting solution was cooled to rt and allowed to stand for 2 h. The colorless crystalline material that resulted was collected by filtration and washed with ice cold MeOH (10 mL) to give the title compound (5.4 g, 71%). MS (ESI): mass calcd. for C4H5ClN4, 144.0; m/z found, 145.0 [M+H]+. 1H NMR ((CD3)250): 7.64 (s, 1H), 6.70 (s, 2H), 4.93 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440978B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-6fbcc52a42154b628a7afb18ebbb138a |
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| 出典メモ | uspto-grants-2016_09 |
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