Hydrochloric Acid → 8-Chloro-4-(4-methoxyphenyl)-3-oxoquinoxaline-2-carboxylic acid

HRID 240356ノート

反応式

HRID 240356 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[N:4]=[C:5]([C:21]([O:23]CC)=[O:22])[C:6](=[O:20])[N:7]2[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1.[OH-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[N:4]=[C:5]([C:21]([OH:23])=[O:22])[C:6](=[O:20])[N:7]2[C:12]1[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67533339Des-(2-cyclohexane-1,3-dione) Fenquinotrione Ethyl Ester

生成物 1

HCID 675332908-Chloro-4-(4-methoxyphenyl)-3-oxoquinoxaline-2-carboxylic acid収率 94.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

7.7 g (21.5 mmol) of ethyl 5-chloro-1-(4-methoxyphenyl)-2-oxo-1,2-dihydroquinoxaline-3-carboxylate was dissolved in ethanol (100 ml), and 6.9 g (43.1 mmol) of a 25% aqueous solution of sodium hydroxide was added thereto. The mixture was stirred for 12 hours at room temperature. The reaction mixture was concentrated under reduced pressure, water was added to the residue thus obtained, and the mixture was acidified using 10% hydrochloric acid. A solid precipitated therefrom was separated by filtration, washed with water, and then dried, to obtain 6.7 g (yield: 94%) of 5-chloro-1-(4-methoxyphenyl)-2-oxo-1,2-dihydroquinoxaline-3-carboxylic acid as a pale yellow powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, water
  2. additionwas added to the residue
  3. customthus obtained
  4. customA solid precipitated
  5. customtherefrom was separated by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-ebdf7b0fa55f45409467858eff7113dd
出典データセット
uspto-grants-2014_02
特許番号
US08648075B2

反応ノート

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