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HCID 18925402、化合物 → HCID 18925404、化合物

HRID 1289076
ノート
印刷プレビュー

反応式

HRID 1289076 の反応式
[N+:1]([C:4]1[CH:8]=[CH:7][S:6][C:5]=1[C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=1)([O-])=O>[Fe].C(O)(=O)C>[NH2:1][C:4]1[CH:8]=[CH:7][S:6][C:5]=1[C:9]1[CH:10]=[CH:11][C:12]([Cl:15])=[CH:13][CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 18925402HCID 18925402、化合物

生成物 1

HCID 18925404HCID 18925404、化合物収率 62%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

To 20 ml of acetic acid, 1 g of 3-nitro-2-(4-chlorophenyl)thiophene and 0.93 g of iron powder were added and heated for 2 hours at 60° C. The reaction mixture was filtered through a diatomaceous earth (Celite) layer. Ethyl acetate was added to the filtrate and extracted 5 times with a 5% aqueous hydrogen chloride solution. The aqueous layer was neutralized with sodium hydrogen carbonate and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 0.54 g of the product as an yellow brown crystal. The yield was 62%. 1H-NMR(CDCl3, δ value):3.82(2H, brs), 6.64(1H, d, J=5.1), 7.12(1H, d, J=5.1), 7.34-7.39(2H, m), 7.43-7.48(2H, m)

後処理

  1. filtrationThe reaction mixture was filtered through a diatomaceous earth (Celite) layer
  2. additionEthyl acetate was added to the filtrate
  3. extractionextracted 5 times with a 5% aqueous hydrogen chloride solution
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-2a92a78c2bba40a8944d5cacdaaf4156
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05747518

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート