化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 6-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chloroaniline | HCID 7812 | — |
| 反応物 | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine | HCID 16726311 | 99.8% |
反応手順
5-amino-4,6-dichloropyrimidine (5.00 g, 29 mmol) and 4-chloroaniline (4.71 g, 36 mmol) were suspended in 80 ml H2O and 12 ml ethanol. Concentrated HCl (1.2 ml, 14.5 mmol) was added at room temperature followed by warming reaction to 82° C. After stirring for 19 hours the reaction was cooled to room temperature and stirred for 60 hours. The precipitate was collected on a sintered glass funnel and rinsed with water followed by hexanes. After drying under vacuum, I-(1A-1)a was obtained as an off-white solid (7.38 g, 98%): +ESI MS (M+1) 255.3; 1H NMR: (400 MHz, CD3OD): δ 7.87 (s, 1H), 7.66 (d, J=8.7 Hz, 2 H), 7.30 (d, J=8.7 Hz, 2 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129239B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-93a9f1f639764b5b8afb51c603527d38 |
| 出典メモ | uspto-grants-2006_10 |