Trifluoroacetic acid → Methyl 6-amino-4-bromopyridine-2-carboxylate

HRID 1725482노트

반응식

HRID 1725482 반응식
[Br:1][C:2]1[CH:7]=[C:6]([NH:8]C(OC(C)(C)C)=O)[N:5]=[C:4]([C:16]([O:18][CH3:19])=[O:17])[CH:3]=1.FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[NH2:8][C:6]1[N:5]=[C:4]([C:16]([O:18][CH3:19])=[O:17])[CH:3]=[C:2]([Br:1])[CH:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 25067269Methyl 4-bromo-6-[(tert-butoxycarbonyl)amino]pyridine-2-carboxylate

생성물 1

HCID 29919299Methyl 6-amino-4-bromopyridine-2-carboxylate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

7.23 g of methyl 4-bromo-6-t-butoxycarbonylamino-pyridine-2-carboxylate was dissolved in 30 ml of chloroform, and then 15 ml of trifluoroacetic acid was added thereto, followed by stirring at room temperature for 1 hour. After concentrating the reaction mixture, the residue was dissolved in ethyl acetate and washed with saturated sodium bicarbonate and brine. The organic layer was dried over anhydrous magnesium sulfate, filtered, and then concentrated in vacuo. The residue was purified by a silica gel column chromatography (eluent: chloroform to chloroform/methanol=20/1) to give the title compound.

후처리

  1. concentrationAfter concentrating the reaction mixture
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with saturated sodium bicarbonate and brine
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by a silica gel column chromatography (eluent: chloroform to chloroform/methanol=20/1)

출처 및 근거

ORD 기록
ord-91e3626e3eda4642a651e40e6562093a
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07491720B2

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