Tetrahydrofuran → 2-(Ethyl(1-ethynylcyclohexyl)amino)ethan-1-ol

HRID 347213

반응식

HRID 347213 반응식
[CH2:1]([NH:3][CH:4](O)[CH3:5])[CH3:2].C(O[C:11]1([C:17]#[CH:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)(=O)C.C1C[O:22]CC1>Cl[Cu]>[CH2:1]([N:3]([C:11]1([C:17]#[CH:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)[CH2:4][CH2:5][OH:22])[CH3:2]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 78903Cyclohexanol, 1-ethynyl-, 1-acetateHCID 18179409Ethylaminoethanol

생성물 1

HCID 223141892-(Ethyl(1-ethynylcyclohexyl)amino)ethan-1-ol

시약·촉매·용매 1

HCID 62652Cuprous chloride촉매

실험 절차

To 1.17 ml (12 mmo) ethylaminoethanol in 8 ml THF were added 29.8 mg (0.3 mmol) CuCl, followed by 1 g (6.02 mmol) 1-ethynylcyclohexyl acetate. The solution was stirred at RT for 3 h, the solvent was removed and the residue dissolved in ether/2M HCl. The phases were separated, and after addition of NaOH (pH11) to the aqueous phase, it was extracted with ether. The ether phase was dried over Na2SO4 and concentrated. Distillation by Kugelrohr yielded 2-[Ethyl-(1-ethynyl-cyclohexyl)-amino]-ethanol as colorless oil, MS: 196 (MH+).

후처리

  1. customthe solvent was removed
  2. dissolutionthe residue dissolved in ether/2M HCl
  3. customThe phases were separated
  4. additionafter addition of NaOH (pH11) to the aqueous phase, it
  5. extractionwas extracted with ether
  6. dry with materialThe ether phase was dried over Na2SO4
  7. concentrationconcentrated
  8. distillationDistillation by Kugelrohr

출처 및 근거

ORD 기록
ord-812a42b562b4483992146eccdf850e9a
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07173043B2

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