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

HRID 1091844

반응식

HRID 1091844 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-8c6ce5e83fbe45a1bfd00fde849a74c2
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129401B2

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