Trifluoroacetic acid → (2-Chloro-4-iodo-pyridin-3-yl)-methyl-amine

HRID 878242노트

반응식

HRID 878242 반응식
C(O[C:6](=O)[N:7]([C:9]1[C:10]([Cl:16])=[N:11][CH:12]=[CH:13][C:14]=1[I:15])C)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:16][C:10]1[C:9]([NH:7][CH3:6])=[C:14]([I:15])[CH:13]=[CH:12][N:11]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 86670802(2-Chloro-4-iodo-pyridin-3-yl)-methyl-carbamic acid tert-butyl ester

생성물 1

HCID 86670801(2-Chloro-4-iodo-pyridin-3-yl)-methyl-amine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To an ice-cold solution of (2-chloro-4-iodo-pyridin-3-yl)-methyl-carbamic acid tert-butyl ester (0.97 g, 2.63 mmol) in CH2Cl2 (5 mL) was added TFA (6.00 g, 4.05 mL, 52.6 mmol) and the solution was stirred at room temperature for 1.5 hours before another TFA (6.00 g, 4.05 mL, 52.6 mmol) was added. After stirring at room temperature for 3 hours the clear solution was evaporated. The residue was taken up in saturated aqueous NaHCO3 solution (50 mL) and CH2Cl2 (30 mL) and the layers were separated. The aqueous layer was extracted twice with CH2Cl2 (30 mL each) and the organic layers were washed with brine, dried over MgSO4, filtered and evaporated. Colorless oil (0.61 g; 86%). MS (ESI): m/z=268.93 [M+H]+.

후처리

  1. additionwas added
  2. customwas evaporated
  3. customCH2Cl2 (30 mL) and the layers were separated
  4. extractionThe aqueous layer was extracted twice with CH2Cl2 (30 mL each)
  5. washthe organic layers were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-bfcd0a3ac72d407d8bf238f0fe4c4df4
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987307B2

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