Potassium Hydroxide → 3-Methyl-6,7-bis(phenylmethoxy)quinoxaline-2-carboxylic acid

HRID 37363노트

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HRID 37363 반응식
[CH3:1][C:2]1[C:3]([C:28]([O:30]CC2C=CC=CC=2)=[O:29])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[C:7]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH:6]=2.[OH-].[K+]>C(O)C.O>[CH3:1][C:2]1[C:3]([C:28]([OH:30])=[O:29])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([O:12][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)=[C:7]([O:20][CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[CH:6]=2

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 867476253-Methyl-6,7-bis(phenylmethoxy)quinoxaline-2-carboxylic acid, phenylmethyl ester

생성물 1

HCID 214584733-Methyl-6,7-bis(phenylmethoxy)quinoxaline-2-carboxylic acid

시약·촉매·용매 1

HCID 19096565Water ethanol용매

반응 조건

온도
80 °C

실험 절차

The compound of Example 27A (4.9 g, 10.0 mmol) was added to a solution of potassium hydroxide (2.2 g, 40.0 mmol) in ethanol/water (80 ml/16 ml) and the mixture was stirred at 80° C. for 20 hours and then cooled (5° C.). The precipitate was collected by suction, washed with ether (4.3 g) and then suspended in water (100 ml). After correction of the pH of this suspension to 2 by the addition of 2N HCl stirring was continued at room temperature for 20 minutes and the crystallized title compound was isolated by suction, washed with water and dried in vacuo over P2O5. Yield: 3.4 g (85%); mp 198°-200° C. C24H20N2O4 0.1 H2

후처리

  1. temperaturecooled (5° C.)
  2. customThe precipitate was collected by suction
  3. washwashed with ether (4.3 g)
  4. additionAfter correction of the pH of this suspension to 2 by the addition of 2N HCl stirring
  5. waitwas continued at room temperature for 20 minutes
  6. customthe crystallized title compound
  7. customwas isolated by suction
  8. washwashed with water
  9. dry with materialdried in vacuo over P2O5

출처 및 근거

ORD 기록
ord-c946305e6dd04a378af5d854d5b55041
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420277

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