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

HRID 2228845
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HRID 2228845 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 21645Hydroxylamine HClHCID 54346298HCID 54346298, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 1049Pyridine용매

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온도
23 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-adaeb010e171493b90c79b95123bf649
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06417388B1

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