Sodium Hydroxide → HCID 86652761, 화합물

HRID 453930노트

반응식

HRID 453930 반응식
[CH:1]1([O:6][C:7]2[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:8]=2[CH:9]=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[NH2:18][OH:19].[OH-].[Na+]>C(O)C>[CH:1]1([O:6][C:7]2[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:8]=2[CH:9]=[N:18][OH:19])[CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 6484666HCID 6484666, 화합물

생성물 1

HCID 86652761HCID 86652761, 화합물수율 97.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To the stirred solution of 2-(cyclopentyloxy)-3-methoxybenzaldehyde (3 g, 13.636 mmol) in ethanol was added hydroxylamine hydrochloride (1.758 g, 27.277 mmol) and aqueous solution of sodium hydroxide (18 ml, 34.091 mmol). The reaction mixture was refluxed for 6 h under nitrogen atmosphere. The solvent was evaporated under reduced pressure and the reaction mixture diluted with water. The product was extracted using chloroform (3×200 ml), combined organic layers washed with water (3×100 ml), brine (50 ml), dried (Na2SO4), filtered and concentrated under vacuum to yield 3.12 g of the product. 1H NMR (300 MHz, CDCl3) δ 1.58-1.64 (m, 4H), 1.66-1.72 (m, 4H), 3.84 (s, 3H), 4.86 (br s, 1H), 6.89 (d, J=8.1 Hz, 1H), 6.99 (t, J=7.8 Hz, 1H), 7.31 (d, J=7.8 Hz, 1H), 8.43 (s, 1H).

후처리

  1. temperatureThe reaction mixture was refluxed for 6 h under nitrogen atmosphere
  2. customThe solvent was evaporated under reduced pressure
  3. additionthe reaction mixture diluted with water
  4. extractionThe product was extracted
  5. washwashed with water (3×100 ml), brine (50 ml)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-6d899aa9929c4ee39f4ebd274987225a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492568B2

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