Sodium Carbonate → (R)-2,2-dimethyl-1,3-dioxolane-4-carbaldehyde oxime

HRID 1511138노트

반응식

HRID 1511138 반응식
[CH3:1][C:2]1([CH3:10])[O:6][C@H:5]([C:7](=O)C)[CH2:4][O:3]1.Cl.[NH2:12][OH:13].C([O-])([O-])=O.[Na+].[Na+]>C1COCC1>[CH3:1][C:2]1([CH3:10])[O:6][C@H:5]([CH:7]=[N:12][OH:13])[CH2:4][O:3]1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 188603Ethanone, 1-(2,2-dimethyl-1,3-dioxolan-4-yl)-, (S)-HCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 86644159(R)-2,2-dimethyl-1,3-dioxolane-4-carbaldehyde oxime수율 97.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (S)-1-(2,2-dimethyl-1,3-dioxolan-4-yl)ethanone (10.5 g, 72.8 mmol) in 150 (mL) THF: 60 mL was added hydroxylamine hydrochloride (5.06 g, 72.8 mmol), and the reaction was stirred for 20 minutes. Na2CO3 (3.78 g, 35.7 mmol) was added and the reaction was stirred overnight. The reaction was extracted with ethyl acetate, washed with water and brine, dried over MgSO4, filtered and concentrated to afford (R)-2,2-dimethyl-1,3-dioxolane-4-carbaldehyde oxime (10.3 g, 71.0 mmol, 97.4% yield).

후처리

  1. stirringthe reaction was stirred overnight
  2. extractionThe reaction was extracted with ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c71e3e1b921f4e27b3934633b83a8eee
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08212045B2

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