Water → HCID 18466731、化合物

HRID 368365ノート

反応式

HRID 368365 の反応式
[CH:1]([C:4]1[C:13]([CH:14]([CH3:16])[CH3:15])=[N:12][C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=1)([CH3:3])[CH3:2].[OH2:17]>C(O)(=O)C>[CH:1]([C:4]1[C:13]([CH:14]([CH3:16])[CH3:15])=[N:12][C:11]2[CH2:10][CH2:9][CH2:8][C:7](=[O:17])[C:6]=2[N:5]=1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 962Water2 回HCID 18466650HCID 18466650、化合物

生成物 1

HCID 18466731HCID 18466731、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
80 °C

実験手順

1.5 g of 5,6,7,8-tetrahydro-2,3-diisopropyl-quinoxaline was dissolved in 10 ml of acetic acid, followed by the dropwise addition of a solution of 1.0 g of chromic acid anhydride in acetic acid (6 ml)/water (1 ml). The obtained mixture was stirred at 80° C. for 2 hours, cooled by allowing to stand, and poured into water, followed by the extraction with ethyl acetate. The organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate, and concentrated in a vacuum. The obtained residue was purified by silica gel chromatography (developer: 10% ethyl acetate/hexane) to give 0.6 g of the title compound as a brown solid.

後処理

  1. temperaturecooled
  2. extractionfollowed by the extraction with ethyl acetate
  3. washThe organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate
  4. dry with materiala saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in a vacuum
  6. customThe obtained residue was purified by silica gel chromatography (developer: 10% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-28bcc01c5b984339be435b8b4a4942aa
出典データセット
uspto-grants-2000_10
特許番号
US06133283

反応ノート

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