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Hydroxylamine HCl → 5-methylhex-5-en-2,3-dione 3-(O-methyloxime) 2-oxime

HRID 2228845
ノート
印刷プレビュー

反応式

HRID 2228845 の反応式
[CH3:1][O:2][N:3]=[C:4]([CH2:8][C:9]([CH3:11])=[CH2:10])[C:5](=O)[CH3:6].[Cl-].[OH:13][NH3+:14]>CO.O.N1C=CC=CC=1>[CH3:1][O:2][N:3]=[C:4]([CH2:8][C:9]([CH3:11])=[CH2:10])[C:5](=[N:14][OH:13])[CH3:6]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 21645Hydroxylamine HClHCID 54346298HCID 54346298、化合物

生成物 1

HCID 1363835465-methylhex-5-en-2,3-dione 3-(O-methyloxime) 2-oxime

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 1049Pyridine溶媒

反応条件

温度
23 °C

実験手順

283.4 g of 5-methylhex-5-ene-2,3-dione 3-(O-methyloxime) in 800 ml of methanol were added dropwise to the solution of 140.6 g of hydroxylammonium chloride in 400 ml of water and 216.7 g of pyridine, and the mixture was stirred at 23° C. for 3 hours. The solvent was then removed under reduced pressure and the residue was poured into ice-water. The pH was subsequently adjusted to 1 using 20% strength sulfuric acid, and the precipitated product was filtered off with suction, taken up in methyl tert-butyl ether and washed with water. The organic phase was then dried over sodium sulfate and the solvent was removed under reduced pressure. This gave 266 g of the title compound as a colorless solid.

後処理

  1. customThe solvent was then removed under reduced pressure
  2. additionthe residue was poured into ice-water
  3. filtrationthe precipitated product was filtered off with suction
  4. washwashed with water
  5. dry with materialThe organic phase was then dried over sodium sulfate
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-adaeb010e171493b90c79b95123bf649
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06417388B1

反応ノート

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