Water → methyl 4-nitro-1H-indazole-1-carboxylate

HRID 451595ノート

反応式

HRID 451595 の反応式
[H-].[Na+].[N+:3]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH:8]=[N:9][NH:10]2)([O-:5])=[O:4].Cl[C:16]([O:18][CH3:19])=[O:17].O>CN(C=O)C>[N+:3]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH:8]=[N:9][N:10]2[C:16]([O:18][CH3:19])=[O:17])([O-:5])=[O:4]

参加物

6

反応物 4

HCID 962WaterHCID 6586Methyl chloroformateHCID 180574-NitroindazoleHCID 24758Sodium hydride

生成物 1

HCID 22032604methyl 4-nitro-1H-indazole-1-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

NaH (0.3 g, 12.5 mmol) in DMF (5 mL) was treated with 4-nitro-1H-indazole (1.33 g, 10 mmol) at 0° C. The reaction mixture was allowed to warm to room temperature and stir for 1 hour. The mixture was treated with methyl chloroformate (0.9 mL) and stirred at room temperature for 3 hours. The mixture was treated with water and filtered to provide the title compound as a solid. 1H NMR (300 MHz, DMSO-d6) δ 4.19 (s, 3H), 7.9 (t, 1H), 8.38 (d, 1H), 8.62 (d, 1H), 8.85 (s, 1H).

後処理

  1. stirringstirred at room temperature for 3 hours
  2. filtrationfiltered

出典と根拠

ORDレコード
ord-dbeb60ad40da48e7b72131fd2bb76c97
出典データセット
uspto-grants-2013_07
特許番号
US08487116B2

反応ノート

読み込み中…