Trifluoroacetic acid → [3-(3-Fluorophenyl)-1H-5-indazolyl]methanamine

HRID 503134

반응식

HRID 503134 반응식
[NH2:1][CH2:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8](C(OC(C)(C)C)=O)[N:7]=[C:6]2[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[F:25][C:21]1[CH:20]=[C:19]([C:6]2[C:5]3[C:9](=[CH:10][CH:11]=[C:3]([CH2:2][NH2:1])[CH:4]=3)[NH:8][N:7]=2)[CH:24]=[CH:23][CH:22]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 222606941h-Indazole-1-carboxylic acid,5-(aminomethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester

생성물 1

HCID 22260728[3-(3-Fluorophenyl)-1H-5-indazolyl]methanamine수율 88.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 300 mg of tert-butyl 5-(aminomethyl)-3-(3-fluorophenyl)-1H-1-indazolecarboxylate in 1 ml methylene chloride was added 2 ml of trifluoroacetic acid, and the mixture was stirred at room temperature for 6.5 hours. After removing the solvent by filtration, to the residue was added 20 ml of ethyl acetate. The mixture was sequentially washed with saturated aqueous sodium hydrogencarbonate solution (×2) and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 188 mg of the title compound as yellow crystals.

후처리

  1. customAfter removing the solvent
  2. filtrationby filtration
  3. additionto the residue was added 20 ml of ethyl acetate
  4. washThe mixture was sequentially washed with saturated aqueous sodium hydrogencarbonate solution (×2) and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-144956c593204410bf9a8b80913c8a9b
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776890B2

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