Cyanoacetic acid → (7-Methoxy-1-benzofuran-3-yl)acetonitrile

HRID 548982

反応式

HRID 548982 の反応式
[CH3:1][O:2][C:3]1[C:11]2[O:10][CH2:9][C:8](=O)[C:7]=2[CH:6]=[CH:5][CH:4]=1.[C:13]([CH2:15]C(O)=O)#[N:14].C([O-])(=O)C.[NH4+]>C1(C)C(C)=CC=CC=1>[CH3:1][O:2][C:3]1[C:11]2[O:10][CH:9]=[C:8]([CH2:15][C:13]#[N:14])[C:7]=2[CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 9740Cyanoacetic acidHCID 517165Ammonium AcetateHCID 28181127-Methoxybenzofuran-3(2H)-one

生成物 1

HCID 15618729(7-Methoxy-1-benzofuran-3-yl)acetonitrile収率 30%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

The solution of 7-methoxy-1-benzofuran-3(2H)-one (reference) (7.5 g, 0.046 mol), cyanoacetic acid (19.55 g, 0.23 mol) and ammonium acetate (7.08 g, 0.092 mol) in xylene was refluxed for 16-18 h. using dean stark apparatus. Xylene was removed under diminished pressure. Brown black residue was taken in ethyl acetate, washed with water and concentrated. On purification on silica gel it yielded (7-methoxy-1-benzofuran-3-yl)acetonitrile (30%).

後処理

  1. customXylene was removed under diminished pressure
  2. washwashed with water
  3. concentrationconcentrated
  4. customOn purification on silica gel it

出典と根拠

ORDレコード
ord-ac3f40c2faa7422a8e9aaa0d2bc845a9
出典データセット
uspto-grants-2011_05
特許番号
US07943634B2

関連ノート

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