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

HRID 557131

反応式

HRID 557131 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 24593copper(I) bromide触媒HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-750182114b4e45759498917073504d29
出典データセット
uspto-grants-2011_11
特許番号
US08058431B2

関連ノート

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