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

HRID 72199
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반응식

HRID 72199 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-8eb6000f04664cc7b29ae986b959446c
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08828991B2

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