Sodium Hydroxide → 2-[1-(Ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)cyclohex-2-en-1-one

HRID 978977

반응식

HRID 978977 반응식
Cl.[CH2:2]([O:4][NH2:5])[CH3:3].[OH-].[Na+].[OH:8][C:9]1[CH2:14][CH:13]([C:15]2[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[C:17]([N+:23]([O-:25])=[O:24])[C:16]=2[CH3:26])[CH2:12][C:11](=[O:27])[C:10]=1[C:28](=O)[CH2:29][CH3:30]>C(O)C>[CH2:2]([O:4][N:5]=[C:28]([C:10]1[C:11](=[O:27])[CH2:12][CH:13]([C:15]2[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[C:17]([N+:23]([O-:25])=[O:24])[C:16]=2[CH3:26])[CH2:14][C:9]=1[OH:8])[CH2:29][CH3:30])[CH3:3]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 76850O-ethylhydroxylamine hydrochlorideHCID 178458845HCID 178458845, 화합물

생성물 1

HCID 1362095012-[1-(Ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)cyclohex-2-en-1-one수율 83.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethoxyamine hydrochloride (0.26 g; 2.7 mmole) and then sodium hydroxide (0.11 g; 2.7 mmole) were added to a solution of 3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)-2-propionylcyclohex-2-en-1-one (0.6 g; 1.8 mmole) in absolute ethanol (150 ml). The mixture was stirred at room temperature for a period of 18 hours and then the ethanol was removed by evaporation under reduced pressure. The residue was treated with dichloromethane and the organic phase was washed twice with water and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure to give the product, 2-[1-(ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)cyclohex-2-en-1-one (0.56 g; 83.2%) as a pale yellow oil. The product was characterized by proton nuclear magnetic resonance spectroscopy and the spectroscopic data is recorded in Table 5, Example 37.

후처리

  1. customthe ethanol was removed by evaporation under reduced pressure
  2. additionThe residue was treated with dichloromethane
  3. washthe organic phase was washed twice with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-490a3ea9ba4a4cbb8932f83e9356eb32
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666510

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