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

HRID 912928ノート

反応式

HRID 912928 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-665eae0618b741898b96f7ddb3b9fefe
出典データセット
uspto-grants-2011_09
特許番号
US08026241B2

反応ノート

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