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

HRID 548982

반응식

HRID 548982 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-ac3f40c2faa7422a8e9aaa0d2bc845a9
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943634B2

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