関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Pyrimidin-5-amine | HCID 344373 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 2-Chloro-N-pyrimidin-5-yl-acetamide | HCID 20208139 | — |
反応手順
5-Aminopyrimidine (450 mg) was suspended in DCE (2 mL) and acetonitrile (2 mL) in a microwave vial. Chloroacetyl chloride (0.377 mL) was added with stirring. The vial was sealed and the reaction mixture was heated in the microwave at 80° C. for 5 minutes. The solid was filtered off, washed with acetonitrile (2×5 mL), DCE (2×5 mL) and pentane (2 ×30 mL) and then partioned between saturated sodium bicarbonate and DCE (50 mL/50 mL) ensuring the aqueous layer was still basic. The organic layer was separated and the aqueous layer was extracted with DCE (2×75 mL). The combined organic layer was dried over magnesium sulfate and evaporated to give the sub-titled compound (200 mg) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08329729B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-4a31dca5b97042f5afd384119e29a258 |
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| 出典メモ | uspto-grants-2012_12 |
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