2-Bromo-5-methoxybenzoic acid → 6-methoxy-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

HRID 557131

반응식

HRID 557131 반응식
Br[C:2]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[O-:13][C:14]#[N:15].[K+]>N1C=CC=CC=1.[Cu]Br>[CH3:12][O:11][C:8]1[CH:9]=[CH:10][C:2]2[NH:15][C:14](=[O:13])[O:6][C:4](=[O:5])[C:3]=2[CH:7]=1

참가 물질

5

반응물 2

HCID 899062-Bromo-5-methoxybenzoic acidHCID 11378442Potassium cyanate

생성물 1

HCID 2944796-methoxy-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

시약·촉매·용매 2

HCID 24593copper(I) bromide촉매HCID 1049Pyridine용매

실험 절차

5.00 g (21.6 mmol) 2-Bromo-5-methoxy-benzoic acid, 620 mg (4.32 mmol) copper (I) bromide and 2.63 g (32.4 mmol) potassium cyanate were dissolved in pyridine and boiled for 30 min. The solvent was removed and the residue was dissolved in 150 ml 2N hydrogen chloride acid and 150 ml ethyl acetate. The organic solvent was treated with water and brine, dried over magnesium sulfate and removed. The residue was digested with methanol.

후처리

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in 150 ml 2N hydrogen chloride acid
  3. additionThe organic solvent was treated with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customremoved

출처 및 근거

ORD 기록
ord-750182114b4e45759498917073504d29
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058431B2

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