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

HRID 725248ノート

反応式

HRID 725248 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb5e63b0a78a4ab1baea0f2e61bd171d
出典データセット
uspto-grants-1998_01
特許番号
US05705645

反応ノート

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