Water → HCID 18466731, 화합물

HRID 368364노트

반응식

HRID 368364 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18466731HCID 18466731, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-351fa414d4a94665ba0690d25124a244
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133283

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