関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-(3,5-Difluoro-4-nitro-phenyl)-morpholine | HCID 66862154 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,6-Difluoro-4-morpholin-4-yl-phenylamine | HCID 59244384 | 90% |
反応手順
Concentrated hydrochloric acid (4.2 mL) was added slowly to a mixture of zinc dust (3.3 g) and 4-(3,5-difluoro-4-nitro-phenyl)-morpholine (2.49 g) in tetrahydrofuran (40 mL) cooled to 0° C. The reaction mixture was then stirred for 1 hour at 0° C. and 2 hours at 25° C. The reaction mixture was filtered through Celite (10 g), concentrated in vacuo and purified by flash chromatography to furnish 1.96 g (90% yield) of the title compound as a white solid. GC-MS (fez) 214 (M); tR=5.83. 1H NMR (500 MHz, DMSO-d6): 2.94 (t, 4H), 3.69 (t, 4H), 4.53 (s, 2H), 6.57 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07812023B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-23050239762b4eac89f0644338fe1295 |
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| 出典メモ | uspto-grants-2010_10 |
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