Trifluoroacetic acid → 4-Iodo-5-methylpyridin-2-amine

HRID 537030노트

반응식

HRID 537030 반응식
COC1C=C(OC)C=CC=1C[NH:6][C:7]1[CH:12]=[C:11]([I:13])[C:10]([CH3:14])=[CH:9][N:8]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[I:13][C:11]1[C:10]([CH3:14])=[CH:9][N:8]=[C:7]([NH2:6])[CH:12]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66747638N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine

생성물 1

HCID 667478634-Iodo-5-methylpyridin-2-amine수율 75%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of N-(2,4-dimethoxybenzyl)-4-iodo-5-methylpyridin-2-amine (118 g, 310 mmol) in DCM (1900 mL) was added TFA (360 mL, 4830 mmol). The reaction mixture was allowed to stir at rt for 2 h and was then concentrated. The residue was dissolved in EtOAc and diluted with saturated aqueous NaHCO3. The mixture was extracted with EtOAc. The organic solutions were combined, washed with brine, dried over Na2SO4, filtered and concentrated to give 4-iodo-5-methylpyridin-2-amine (53 g, 75%) which was used in the next step without purification.

후처리

  1. concentrationwas then concentrated
  2. dissolutionThe residue was dissolved in EtOAc
  3. additiondiluted with saturated aqueous NaHCO3
  4. extractionThe mixture was extracted with EtOAc
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-53c9cc6ca31e48b7a5fe269bf9f6357e
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859768B2

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