Potassium Carbonate → Ethyl 3-amino-6-nitro-1-benzothiophene-2-carboxylate

HRID 43797

反応式

HRID 43797 の反応式
[N+]([C:4]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:5]=1[C:6]#[N:7])([O-])=O.C(=O)([O-])[O-].[K+].[K+].[C:21]([O:25][CH2:26][CH3:27])(=[O:24])[CH2:22][SH:23]>CN(C=O)C>[NH2:7][C:6]1[C:5]2[CH:8]=[CH:9][C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:4]=2[S:23][C:22]=1[C:21]([O:25][CH2:26][CH3:27])=[O:24]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12185Ethyl ThioglycolateHCID 5540822,4-Dinitrobenzonitrile

生成物 1

HCID 67549245Ethyl 3-amino-6-nitro-1-benzothiophene-2-carboxylate収率 32.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2,4-Dinitrobenzonitrile (5.08 g, 26.3 mmol) was dissolved in DMF (55 ml). Potassium carbonate (4.36 g, 31.6 mmol) and ethyl thioglycolate (3.17 g, 26.3 mmol) were added, and the mixture was stirred at room temperature for three days. The reaction solution was concentrated under reduced pressure, diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was recrystallized from ethyl acetate/hexane to obtain 2.27 g of the title compound as crystals (32%).

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additiondiluted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentration under reduced pressure
  6. customthe residue was recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-9fd42774e03b4419938ca01fdb1efa66
出典データセット
uspto-grants-2013_09
特許番号
US08536197B2

関連ノート

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