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

HRID 1741954ノート

反応式

HRID 1741954 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 3283Diethyl Ether溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f2f5b48425ae4ee8a421f980258c31e4
出典データセット
uspto-grants-1994_08
特許番号
US05334740

反応ノート

読み込み中…