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

HRID 1942153노트

반응식

HRID 1942153 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f06b80e39749478dbf469a81494ecf21
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389523B2

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