Hydrazine hydrate (1:1) → HCID 178423887, 화합물

HRID 721984

반응식

HRID 721984 반응식
C[N:2]([CH:4]=[C:5]1[CH2:9][CH2:8][C:7]([CH3:11])([CH3:10])[C:6]1=O)C.O.[NH2:14]N>C(O)C>[CH3:10][C:7]1([CH3:11])[C:6]2[C:5](=[CH:4][NH:2][N:14]=2)[CH2:9][CH2:8]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 695835902-[(Dimethylamino)methylene]-5,5-dimethylcyclopentanone

생성물 1

HCID 178423887HCID 178423887, 화합물수율 102.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-[(dimethylamino)methylene]-5,5-dimethylcyclopentanone (12.5 g, 75 mmol) in ethanol (100 mL) at room temperature was added hydrazine hydrate (4 mL, 82.3 mmol). The reaction mixture was heated at reflux overnight. It was then cooled to room temperature and concentrated. Water (700 mL) was added to the residue, and the resulting solution was extracted twice with diethyl ether (2×250 mL). The organic extracts were combined, dried over MgSO4 and concentrated to give the title compound as an oil (10.5 g). 1H NMR indicated the oil to be ˜60% pure. It was used directly for Step C.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux overnight
  3. concentrationconcentrated
  4. additionWater (700 mL) was added to the residue
  5. extractionthe resulting solution was extracted twice with diethyl ether (2×250 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f657392d3ec74be3a5f9a13e2dda1db6
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138361B2

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