Trifluoroacetic acid → N-(4-iodo-5-methylpyridin-2-yl)cyclopropanecarboxamide

HRID 537029노트

반응식

HRID 537029 반응식
COC1C=C(OC)C=CC=1C[N:6]([C:12]1[CH:17]=[C:16]([I:18])[C:15]([CH3:19])=[CH:14][N:13]=1)[C:7]([CH:9]1[CH2:11][CH2:10]1)=[O:8].C(O)(C(F)(F)F)=O>C(Cl)Cl>[I:18][C:16]1[C:15]([CH3:19])=[CH:14][N:13]=[C:12]([NH:6][C:7]([CH:9]2[CH2:11][CH2:10]2)=[O:8])[CH:17]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66747562N-(2,4-dimethoxybenzyl)-N-(4-iodo-5-methylpyridin-2-yl)cyclopropanecarboxamide

생성물 1

HCID 66748424N-(4-iodo-5-methylpyridin-2-yl)cyclopropanecarboxamide수율 83.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of N-(2,4-dimethoxybenzyl)-N-(4-iodo-5-methylpyridin-2-yl)cyclopropanecarboxamide (1.8 g, 3.95 mmol) in DCM (23 mL) was added TFA. The reaction mixture was allowed to stir at rt overnight and then concentrated. The residue was diluted with DCM and aqueous saturated NaHCO3 and the mixture was extracted with DCM. The organic solutions were combined, dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography to give N-(4-iodo-5-methylpyridin-2-yl)cyclopropanecarboxamide (1.0 g, 75%).

후처리

  1. concentrationconcentrated
  2. additionThe residue was diluted with DCM and aqueous saturated NaHCO3
  3. extractionthe mixture was extracted with DCM
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-3e12a041bb0b4cafa7c1ecfc038fe888
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859768B2

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