3-Methoxyaniline → (3-Methoxy-phenylamino)-phenyl-acetic acid
反応式
Br[CH:2]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:3]([OH:5])=[O:4].[CH3:12][O:13][C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][CH:20]=1)[NH2:17]>C1COCC1>[CH3:12][O:13][C:14]1[CH:15]=[C:16]([NH:17][CH:2]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:3]([OH:5])=[O:4])[CH:18]=[CH:19][CH:20]=1参加物
4
実験手順
A solution of 2-bromo-2-phenylacetic acid (0.5 g, 2.28 mmol) and 3-methoxyaniline (0.54 mL, 4.56 mmol) in THF (12 mL) is refluxed for 4 hours. Solvent is removed under vacuum, the residue is taken up with 1M HCl and extracted with EtOAc. The organic phase is dried (Na2SO4), filtered and evaporated. The crude is purified by flash chromatography (DCM/MeOH=98/2 to 9/1) to obtain intermeaditae I116 as a white solid (0.58 g, 99% yield).
後処理
- customSolvent is removed under vacuum
- extractionextracted with EtOAc
- dry with materialThe organic phase is dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe crude is purified by flash chromatography (DCM/MeOH=98/2 to 9/1)
出典と根拠
- ORDレコード
- ord-d2075340269f4f199e1ba8a3ca303395
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835682B2
反応ノート
読み込み中…