Stannous Chloride → 4-(4-chloro-1H-1,2,3-triazol-1-yl)aniline

HRID 40736ノート

反応式

HRID 40736 の反応式
[Cl:1][C:2]1[N:3]=[N:4][N:5]([C:7]2[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][CH:8]=2)[CH:6]=1.Cl[Sn]Cl>C(O)C>[Cl:1][C:2]1[N:3]=[N:4][N:5]([C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[CH:6]=1

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 687732414-chloro-1-(4-nitrophenyl)-1H-1,2,3-triazole

生成物 1

HCID 595880664-(4-chloro-1H-1,2,3-triazol-1-yl)aniline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

To a solution of 4-chloro-1-(4-nitrophenyl)-1H-1,2,3-triazole (0.1 g, 0.45 mmol) in ethanol (3 mL) was added SnCl2 (0.4 g, 1.8 mmol) portionwise. The slurry was warmed up to 85° C. for 2.5 h, then quenched with NaOH (2M), filtered and concentrated. The residue was redissolved in EtOAc and washed with brine. The organic layer was separated, dried (MgSO4), and concentrated to afford 4-(4-chloro-1H-1,2,3-triazol-1-yl)aniline.

後処理

  1. customquenched with NaOH (2M)
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe residue was redissolved in EtOAc
  5. washwashed with brine
  6. customThe organic layer was separated
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-aa327e72d6a445cda4d6f8ffc6eb3592
出典データセット
uspto-grants-2013_09
特許番号
US08530480B2

反応ノート

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