関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | N'-hydroxy-4-morpholin-4-yl-1,2,5-oxadiazole-3-carboximidamide | HCID 136335830 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-Hydroxy-4-morpholin-4-yl-1,2,5-oxadiazole-3-carboximidoyl chloride | HCID 136335829 | 30% |
反応手順
A solution of N′-hydroxy-4-morpholin-4-yl-1,2,5-oxadiazole-3-carboximidamide (66 mg, 0.3 mmol) in 6.0 M HCl (0.62 mL) at 5-10° C. was treated with a solution of sodium nitrite (32 mg, 0.47 mmol) in water (0.5 mL) dropwise and stirred for 2 h at 0° C. The suspension was filtered and the solid washed with ice water to give desired product (22 mg, 30%). The filtrate was extracted with ethyl acetate (30 mL) which was washed with brine (10 mL), filtered and concentrated to give additional product (23 mg, 32%) that contained minor impurities. The combined material was used immediately 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 | US08372870B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-9afd9b504d79462c93d736cedb0fd9de |
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| 出典メモ | uspto-grants-2013_02 |
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