関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Methyl 6-chloropyridazine-3-carboxylate | HCID 12379801 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Chloropyridazine-3-carboxamide | HCID 12577557 | 99% |
反応手順
Dissolve methyl 6-chloropyridazine-3-carboxylate (0.498 g, 2.89 mmol) in methanol (28 mL). Cool the solution to 0° C. with an acetone/dry ice bath. Bubble ammonia into the reaction mixture then allow it to warm to 0° C. over 1 hour before concentrating to give the title compound (0.451 g, 99%): TOF MS ES+ 157.0 (M)+, HRMS calcd for C5H4N3OCl 157.0043 (M)+, found 157.0010, time 4.45 min; HPLC [YMC-Pro pack C-18 (150×4.6 mm, S-5 microm), 0.1 TFA/acetonitrile in 0.1% TFA/water at 1.0 mL/min, 10-20% over 5 min then 20-95% over 18], tR=5.2 min, 100% purity.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560463B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-74b56fbe96bb4c16b7913c5c79ff1373 |
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| 出典メモ | uspto-grants-2009_07 |
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