Acetic Anhydride → N-(5,6-Dichloro-pyridin-3-ylmethyl)-acetamide

HRID 912928노트

반응식

HRID 912928 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][NH:10]C)[CH:5]=[N:6][C:7]=1[Cl:8].CCN(CC)CC.CC(O[C:23]([CH3:25])=[O:24])=O>CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][NH:10][C:23](=[O:24])[CH3:25])[CH:5]=[N:6][C:7]=1[Cl:8]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 85663685[(5,6-Dichloropyridin-3-yl)methyl](methyl)amine

생성물 1

HCID 19959722N-(5,6-Dichloro-pyridin-3-ylmethyl)-acetamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of the amine from step (c) above (1.77 g, 10 mmol) and Et3N (2.78 mL, 20 mmol, Aldrich) was added Ac2O dropwise with stirring at room temperature. The mixture was stirred for 30 min at room temperature, diluted with EtOAc (30 mL), washed with water (20 mL) and brine (20 mL), dried over Na2SO4, and filtered. The filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography, eluting with 80% EtOAc/hexane to give the title compound. MS (ESI, pos. ion) m/z: 219 (M+1).

후처리

  1. stirringThe mixture was stirred for 30 min at room temperature
  2. washwashed with water (20 mL) and brine (20 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customThe filtrate was evaporated in vacuo
  6. customthe residue was purified by silica gel column chromatography
  7. washeluting with 80% EtOAc/hexane

출처 및 근거

ORD 기록
ord-665eae0618b741898b96f7ddb3b9fefe
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026241B2

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