関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| 反応物 | Trifluoroacetamidine | HCID 2776882 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,2,2-trifluoro-N'-(4-methoxyphenyl)ethanehydrazonamide | HCID 69677622 | 108.3% |
反応手順
To a solution of trifluoroacetoamidine (4.24 g, 37.8 mmol) in methanol (20 mL), were added 4-methoxyphenylhydrazine hydrochloride (4.72 g, 27 mmol) and then triethylamine (3.77 mL, 27 mmol) at room temperature. The mixture was stirred for 6 hours. The solvent was removed under reduced pressure. 20 mL of water and 50 mL of ethyl acetate-tetrahydrofuran (9:1) were added to the residue and the organic layer was separated and the aqueous layer was extracted with 50 mL of ethyl acetate-tetrahydrofuran (9:1). A combined organic layer was washed with water and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure to give 2,2,2-trifluoro-N′-(4-methoxyphenyl)ethanehydrazonamide (6.82 g, 108.2% yield). The residue was used for the next reaction without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06927230B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-46f0bbabc90a4230b8163427f08345aa |
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| 出典メモ | uspto-grants-2005_08 |
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