Hydroxyamine hydrochloride → 4,5-(Dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenal oxime

HRID 1741954노트

반응식

HRID 1741954 반응식
[CH3:1][C:2]1([CH3:17])[O:16][CH:13]([CH:14]=[CH2:15])[CH:4]([CH:5]([O:9][CH2:10][O:11][CH3:12])[CH2:6][CH:7]=O)[O:3]1.Cl.[NH2:19][OH:20]>N1C=CC=CC=1.C(OCC)C>[CH3:1][C:2]1([CH3:17])[O:16][CH:13]([CH:14]=[CH2:15])[CH:4]([CH:5]([O:9][CH2:10][O:11][CH3:12])[CH2:6][CH:7]=[N:19][OH:20])[O:3]1

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 190109744,5-(Dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenal

생성물 1

HCID 730980754,5-(Dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenal oxime수율 91.7%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 3283Diethyl Ether용매

실험 절차

The above 4,5-(dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenal (91.9 mg) was dissolved in 1 ml of pyridine, and 45 mg of hydroxylamine hydrochloride was added at room temperature, and stirring was conducted at room temperature for 8 hours. The reaction mixture was diluted with diethyl ether. The diluted reaction mixture was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to afford 89.5 mg of 4,5-(dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenal oxime having the following properties (yield 52%).

후처리

  1. customThe diluted reaction mixture
  2. washwas washed with a saturated sodium chloride aqueous solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f2f5b48425ae4ee8a421f980258c31e4
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05334740

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