Acetonitrile → 4-Methyl-phenyl-amino-phenyl-acetic acid

HRID 1255080

反応式

HRID 1255080 の反応式
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][C:13]1[CH:18]=[CH:17][C:16](N)=[CH:15][CH:14]=1.C(#[N:22])C>>[CH3:12][C:13]1[CH:18]=[CH:17][C:16]([C:2]([NH2:22])([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:3]([OH:5])=[O:4])=[CH:15][CH:14]=1

参加物

4

反応物 3

HCID 6342AcetonitrileHCID 7813p-ToluidineHCID 97919Bromo(phenyl)acetic acid

生成物 1

HCID 2378904-Methyl-phenyl-amino-phenyl-acetic acid収率 78%

実験手順

To a solution of α-bromophenylacetic acid (1.00 g, 4.65 mmol) in acetonitrile (20 mL), is added 4-methyl-phenylamine (0.96 g, 9.30 mmol) and the mixture reacted in a closed vessel under MW irradiation at 100° C. for 1 hour (UPLC-MS monitoring: complete conversion). Solvent is evaporated and residue is portioned between EtOAc and 2N HCl. The organic phase is dried over Na2SO4, filtered and evaporated to dryness to get desired compound as a yellow solid (0.88 g, 78% yield).

後処理

  1. customthe mixture reacted in a closed vessel under MW irradiation at 100° C. for 1 hour (UPLC-MS monitoring: complete conversion)
  2. customSolvent is evaporated
  3. dry with materialThe organic phase is dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-ae2c1f1f49d84e3a9dc41504bb78270b
出典データセット
uspto-grants-2013_06
特許番号
US08455646B2

関連ノート

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