Water → HCID 18466731、化合物

HRID 368364ノート

反応式

HRID 368364 の反応式
[CH3:1][CH:2]([C:4](=O)[C:5](=O)[CH:6]([CH3:8])[CH3:7])[CH3:3].[CH:11]1([NH2:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH:12]1[NH2:17].[OH2:19]>C(O)(=O)C>[CH:2]([C:4]1[C:5]([CH:6]([CH3:8])[CH3:7])=[N:18][C:11]2[CH2:16][CH2:15][CH2:14][C:13](=[O:19])[C:12]=2[N:17]=1)([CH3:3])[CH3:1]

参加物

5

反応物 3

HCID 962WaterHCID 46101,2-DiaminocyclohexaneHCID 1382172,5-Dimethylhexane-3,4-dione

生成物 1

HCID 18466731HCID 18466731、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

8.7 g of 2,5-dimethyl-3,4-hexanedione and 11.2 ml of 1,2-cyclohexanediamine were dissolved in 20 ml of acetic acid. The obtained solution was heated under reflux for 30 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: 5% ethyl acetate/hexane) to give 6.8 g of the title compound as a colorless oil.

後処理

  1. temperatureThe obtained solution was heated
  2. temperatureunder reflux for 30 hours
  3. temperaturecooled
  4. extractionfollowed by the extraction with ethyl acetate
  5. washThe organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate
  6. dry with materiala saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  7. concentrationconcentrated in a vacuum
  8. customThe obtained residue was purified by silica gel chromatography (developer: 5% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-351fa414d4a94665ba0690d25124a244
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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