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2'-Hydroxyacetophenone → HCID 20560229, 화합물

HRID 1659315
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반응식

HRID 1659315 반응식
[H-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[O:12])[CH3:11].C(O[C:16](=O)[CH2:17][N:18]([CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH3:19])C>O1CCOCC1>[CH2:20]([N:18]([CH2:17][C:16]1[O:3][C:4]2[C:5]([C:10](=[O:12])[CH:11]=1)=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH3:19])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 83752'-HydroxyacetophenoneHCID 24758Sodium hydrideHCID 11031023Ethyl 2-[benzyl(methyl)amino]acetate

생성물 1

HCID 20560229HCID 20560229, 화합물수율 74.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

반응 조건

온도
80 °C

실험 절차

To a suspension of sodium hydride (16.4 g) in absolute dioxane (700 ml) stirred at 80° C., was slowly added a mixture of o-hydroxyacetophenone (31.0 g) and N-benzyl-N-methylglycine ethyl ester (40 g) in dioxane (100 ml), and the resulting solution was boiled for 19 hours before being evaporated in vacuo. The residue was dissolved in ethanol and the mixture was saturated with dry HCl and stirred at room temperature for 18 hours. After evaporation the residue was taken up in chloroform and washed with water. Evaporation of the dried organic extracts yielded an oil (40 g) which was chromatographed on alumina eluting with chloroform to give the title chromone as a yellow oil (17.8 g).

후처리

  1. additionwas slowly added
  2. custombefore being evaporated in vacuo
  3. dissolutionThe residue was dissolved in ethanol
  4. stirringstirred at room temperature for 18 hours
  5. customAfter evaporation the residue
  6. washwashed with water
  7. customEvaporation of the dried organic extracts

출처 및 근거

ORD 기록
ord-4595d5e236714f0b847280a587a8d339
출처 데이터셋
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04303656

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