関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 4,5-Dichloro-2-nitroaniline | HCID 81149 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-2-nitro-5-(1-pyrrolidinyl)aniline | HCID 3613709 | 99% |
反応手順
Pyrrolidine (6 mL) was added to 4,5-dichloro-2-nitro-phenylamine (2.58 g, 12.5 mmol) in a sealed tube and the mixture heated to 100° C. for 6 h. The mixture was cooled to 23° C., poured into water (100 mL) and extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine (50 mL), dried, filtered, and concentrated under reduced pressure to afford the titled compound (3.00 g, 99%). MS (ESI/CI): mass calcd. for C10H12ClN3O2, 241.1; m/z found, 242.1 [M+H]+. 1H NMR (400 MHz, CDCl3): 8.08 (s, 1H), 6.06 (s, 2H), 5.82 (s, 1H), 3.58 (ddd, J=6.6, 4.2, 2.7 Hz, 4H), 2.02-1.90 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08865713B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-c51de608f509485f9149cf8bfd24a5fb |
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| 出典メモ | uspto-grants-2014_10 |
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