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Trifluoroacetic acid → 3-Amino-5-(5-fluoropyridin-2-yl)thiophene-2-carboxylic acid methyl ester

HRID 532423
ノート
印刷プレビュー

反応式

HRID 532423 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][N:19]=2)=[CH:8][C:9]=1[NH:10]C(OC(C)(C)C)=O)=[O:4].FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][N:19]=2)=[CH:8][C:9]=1[NH2:10])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 689429283-tert-Butoxycarbonylamino-5-(5-fluoropyridin-2-yl)thiophene-2-carboxylic acid methyl ester

生成物 1

HCID 689420543-Amino-5-(5-fluoropyridin-2-yl)thiophene-2-carboxylic acid methyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-tert-butoxycarbonylamino-5-(5-fluoropyridin-2-yl)-thiophene-2-carboxylic acid methyl ester (80 mg) in dichloromethane (1.35 mL) was mixed with trifluoroacetic acid (0.15 mL) and stirred at room temperature overnight. The solvent was then removed in vacuo, and the residue was taken up again in dichloromethane and washed twice with saturated NaHCO3 solution and once with water. The dichloromethane phase was dried over sodium sulfate and concentrated. The product with the molecular weight of 252.27 (C11H9FN2O2S) was obtained in this way; MS (ESI): 253 (M+H+).

後処理

  1. customThe solvent was then removed in vacuo
  2. washwashed twice with saturated NaHCO3 solution and once with water
  3. dry with materialThe dichloromethane phase was dried over sodium sulfate
  4. concentrationconcentrated
  5. customThe product with the molecular weight of 252.27 (C11H9FN2O2S) was obtained in this way

出典と根拠

ORDレコード
ord-ddd10b1a79e24a1ab8a1a84e6f920f5d
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853208B2

反応ノート

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