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

HRID 77047

반응식

HRID 77047 반응식
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

참가 물질

4

반응물 3

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

생성물 1

HCID 2378904-Methyl-phenyl-amino-phenyl-acetic acid수율 78%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-78136e439632492782ede2e4ddd841ae
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835682B2

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