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Acetic Acid → 4-bromothieno[2,3-c]pyridine

HRID 2283681
ノート
印刷プレビュー

反応式

HRID 2283681 の反応式
C(O)(=O)C.[Br:5][C:6]1[CH:11]=[N:10][CH:9]=[C:8]2[S:12][C:13](C([O-])=O)=[CH:14][C:7]=12>CN(C=O)C.C(OCC)(=O)C.C(=O)([O-])[O-].[Ag+2]>[Br:5][C:6]1[CH:11]=[N:10][CH:9]=[C:8]2[S:12][CH:13]=[CH:14][C:7]=12
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

6

反応物 2

HCID 176Acetic AcidHCID 131733525HCID 131733525、化合物

生成物 1

HCID 185163464-bromothieno[2,3-c]pyridine

試薬・触媒・溶媒 3

HCID 178418647HCID 178418647、化合物触媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

Silver carbonate (28 mg) and acetic acid (0.006 ml) were added to a solution of 4-bromothieno[2,3-c]pyridine-2-carboxylate obtained in the above-described Step 1 (258 mg) in DMF (2.0 ml), and the reaction solution was stirred at 120° C. for 24 hours. The reaction solution was diluted with ethyl acetate and washed successively with an aqueous sodium bicarbonate solution and a saturated saline solution. After drying over anhydrous sodium sulfate, the solvent was evaporated under vacuum. The resultant residue was purified by column chromatography on silica gel (developing solvent:hexane-ethyl acetate) to obtain 4-bromothieno[2,3-c]pyridine.

後処理

  1. washwashed successively with an aqueous sodium bicarbonate solution
  2. dry with materialAfter drying over anhydrous sodium sulfate
  3. customthe solvent was evaporated under vacuum
  4. customThe resultant residue was purified by column chromatography on silica gel (developing solvent:hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-73a57001af7941ac8f7eb804063eef96
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145414B2

反応ノート

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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