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Diphenyl Ether → HCID 178486804, 화합물

HRID 1517880
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HRID 1517880 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][CH:12]=[C:13]2[C:18](=[O:19])OC(C)(C)OC2=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O(C1C=CC=CC=1)C1C=CC=CC=1>CCCCCC>[CH3:10][O:9][C:8]1[CH:7]=[C:6]2[C:5](=[CH:4][C:3]=1[O:2][CH3:1])[N:11]=[CH:12][CH:13]=[C:18]2[OH:19]
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참가 물질

4

반응물 2

HCID 7583Diphenyl EtherHCID 212340935-[[(3,4-Dimethoxyphenyl)amino]methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione

생성물 1

HCID 178486804HCID 178486804, 화합물수율 95.6%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

5-((3,4-Dimethoxyphenylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (16.1 g, 52 mmol) was added to a pre-heated 1000 mL round-bottom flask containing 1-phenoxy benzene (100 mL) at 230° C. The reaction was stirred for 5 min, and then cooled to 120° C. n-Hexane (100 mL) was added to the solution to allow the product to precipitate out from the reaction solution. The mixture was further stirred at rt overnight. The solid was collected and crystallized in a solution of EtOAc/n-hexane (50 mL, v/v=10/1) to afford the title compound as a brown solid (10.2 g, 95%).

후처리

  1. additionwas added to the solution
  2. customto precipitate out from the reaction solution
  3. stirringThe mixture was further stirred at rt overnight
  4. customThe solid was collected
  5. customcrystallized in a solution of EtOAc/n-hexane (50 mL, v/v=10/1)

출처 및 근거

ORD 기록
ord-ba80023590bd4ddf88cd2f9fc023b57d
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232294B2

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