Hydrochloric Acid → HCID 86681562、化合物
反応式
[F:1][C:2]([F:17])([F:16])[CH2:3][NH:4][C:5]([NH:7][NH:8]C(OC(C)(C)C)=O)=[O:6].[ClH:18]>O1CCOCC1>[ClH:18].[F:1][C:2]([F:17])([F:16])[CH2:3][NH:4][C:5]([NH:7][NH2:8])=[O:6]参加物
4
実験手順
To a stirred solution of tert-butyl 2-((2,2,2-trifluoroethyl)carbamoyl)hydrazinecarboxylate (1.62 g, 6.30 mmol) in anhydrous dioxane (10.0 mL) was added HCl (4M in dioxane, 2-3 mL). The reaction mixture was stirred at ambient temperature for 18 h, then heated at reflux for 2-3 h. The reaction mixture was allowed to cool to ambient temperature and then evaporated to afford the title compound as a white solid (1.33 g, 109%): 1H NMR (400 MHz, DMSO-d6) δ 10.12 (s, 3H), 9.25 (s, 1H), 7.72 (t, J=6.5 Hz, 1H), 3.91 (qd, J=9.7, 6.5 Hz, 2H); 19F NMR (376 MHz, DMSO-d6) δ −71.41; ESIMS m/z 156 ([M−H]−). This material is used without further purification.
後処理
- temperatureheated
- temperatureat reflux for 2-3 h
- temperatureto cool to ambient temperature
- customevaporated
出典と根拠
- ORDレコード
- ord-1c907ab7d2f549108fbe146becdf9a13
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09210927B2
反応ノート
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