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O-ethylhydroxylamine hydrochloride → HCID 136127124, 화합물

HRID 1780619
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인쇄 미리보기

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HRID 1780619 반응식
[CH3:1][C:2]1([CH3:26])[CH2:6][C:5]2[C:7]([CH3:25])=[C:8]([CH3:24])[C:9]([CH:12]3[CH2:17][C:16](=[O:18])[C:15]([C:19](=O)[CH2:20][CH3:21])=[C:14]([OH:23])[CH2:13]3)=[C:10]([CH3:11])[C:4]=2[O:3]1.C([O-])(=O)C.[Na+].Cl.[CH2:33]([O:35][NH2:36])[CH3:34]>C(O)C>[CH3:1][C:2]1([CH3:26])[CH2:6][C:5]2[C:7]([CH3:25])=[C:8]([CH3:24])[C:9]([CH:12]3[CH2:17][C:16](=[O:18])[C:15]([C:19](=[N:36][O:35][CH2:33][CH3:34])[CH2:20][CH3:21])=[C:14]([OH:23])[CH2:13]3)=[C:10]([CH3:11])[C:4]=2[O:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 76850O-ethylhydroxylamine hydrochlorideHCID 517045Sodium AcetateHCID 178458831HCID 178458831, 화합물

생성물 1

HCID 136127124HCID 136127124, 화합물수율 83.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution 0.3 g of the 5-(2,3-dihydro-2,2,4,5,7-pentamethylbenzofuran-6-yl)-2-propionyl-3-hydroxycyclohex-2-en-1-one in 10 ml of ethanol was added 0.14 g of sodium acetate and 0.09 g of ethoxyamine hydrochloric acid. After stirring at room temperature for 20 hours, the reaction mixture was quenched with 20 ml water and extracted with diethyl ether. The combined organic extracts were dried over anhydrous magnesium sulfate, filtered and concentrated under the reduced pressure to afford a crude product. Final purification was carried by silica-gel column chromatography to afford 0.28 g of 5-(2,3-dihydro-2,2,4,5,7-pentamethylbenzofuran-6-yl)-2-[1-(ethoxyimino)propyl]-3-hydroxycyclohex-2-en-1-one as yellow oil.

후처리

  1. customthe reaction mixture was quenched with 20 ml water
  2. extractionextracted with diethyl ether
  3. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under the reduced pressure
  6. customto afford a crude product
  7. customFinal purification

출처 및 근거

ORD 기록
ord-fb17c80804aa4773bb92aa59af637dea
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05631208

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