関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (Phenylmethyl)hydrazine | HCID 11157 | — |
| 反応物 | 2-Oxo-4-phenylbutyric acid | HCID 69732 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 3,4-Dichloro-6-phenylpyridazine | HCID 13163231 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3,4-Dichloro-6-phenylpyridazine | HCID 13163231 | — |
| 生成物 | HCID 13342056 | HCID 13342056 | — |
| 生成物 | 3-Methoxy-4-chloro-6-phenylpyridazine | HCID 66731998 | — |
反応手順
3,4-Dichloro-6-phenylpyridazine was synthesized from □-oxobenzenebutanoic acid and 1-(phenylmethyl)hydrazine in 2 steps according to a procedure by Sircar (Sircar, I. J Het. Chem. 1983, 20,1473-1476.) 3,4-Dichloro-6-phenylpyridazine (100 mg, 0.44 mmol) was combined with sodium methoxide (1.1 mL of a 0.50M solution in methanol, 0.55 mmol, 1.25 equiv.) and methanol (296 μl, 1.5M) in a resealable tube and heated to 65° C. for 1 hour. The methanol was evaporated in vacuo, and water was added to the residue. The mixture was extracted with DCM, dried over K2CO3, filtered and concentrated in vacuo, to afford 3,4-dimethoxy-6-phenylpyridazine and 3-methoxy-4-chloro-6-phenylpyridazine, the title compound, as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560551B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-667bead50e7a433e8d7e7c138df62023 |
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| 出典メモ | uspto-grants-2009_07 |
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