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

HRID 264123ノート

反応式

HRID 264123 の反応式
[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]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 10690735alpha-[[(2,4,6-Trimethoxyphenyl)amino]carbonyl] benzene acetic acid ethyl ester

生成物 1

HCID 10665192alpha-[[(2,4,6-Trimethoxyphenyl)amino]carbonyl]benzene acetic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-81e01f130b4542df8bd5833471c6d736
出典データセット
uspto-grants-1997_07
特許番号
US05646170

反応ノート

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