Potassium Hydroxide → alpha-[[(2,4,6-Trimethoxyphenyl)amino]carbonyl]benzene acetic acid

HRID 1938740노트

반응식

HRID 1938740 반응식
[OH-].[K+].C([O:5][C:6](=[O:29])[CH:7]([C:14]([NH:16][C:17]1[C:22]([O:23][CH3:24])=[CH:21][C:20]([O:25][CH3:26])=[CH:19][C:18]=1[O:27][CH3:28])=[O:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)C>C(O)C.O>[CH3:28][O:27][C:18]1[CH:19]=[C:20]([O:25][CH3:26])[CH:21]=[C:22]([O:23][CH3:24])[C:17]=1[NH:16][C:14]([CH:7]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:6]([OH:29])=[O:5])=[O:15]

참가 물질

5

실험 절차

To a stirred solution of KOH (10.70 g, 0.191 mol) in absolute ethanol (1.1 L) was added α-[[(2,4,6-trimethoxyphenyl)amino]carbonyl] benzene acetic acid ethyl ester (55.28 g, 0.1480 mol), and the mixture was stirred for 41 hours. The resulting suspension was diluted with H2O (~900 mL) and rotoevaporated to remove ethanol. The solution was washed (ethyl acetate) and acidified with dropwise addition of 1M HCl (265 mL). The resulting precipitate was filtered off, washed (H2O), and dried in vacuo to give an off-white solid; yield 48.4 g (100%); 111°-113° C. (gas evolution).

후처리

  1. customto remove ethanol
  2. washThe solution was washed (ethyl acetate)
  3. additionacidified with dropwise addition of 1M HCl (265 mL)
  4. filtrationThe resulting precipitate was filtered off
  5. washwashed (H2O)
  6. customdried in vacuo
  7. customto give an off-white solid
  8. custom111°-113° C. (gas evolution)

출처 및 근거

ORD 기록
ord-00d64589d80e490f90656b58c8590c64
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05693657

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