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HCID 10295973, 화합물 → Diethyl 2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}malonate

HRID 896483
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HRID 896483 반응식
[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:27]=[CH:26][C:13]([CH:14]=[C:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:12][CH:11]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1>O1CCOCC1.[Pd]>[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]([CH2:14][CH:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:26][CH:27]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 10295973HCID 10295973, 화합물

생성물 1

HCID 10159558Diethyl 2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}malonate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

실험 절차

Dissolve the compound obtained in Example 1 (6.7 g) in a dioxane/absolute ethanol mixture (100 ml/20 ml) and add palladium-on-carbon (0.5 g). Stir magnetically at ambient temperature under a hydrogen atmosphere for 76 hours. Remove the palladium-on-carbon by filtration and remove the mixture of solvents by evaporation under reduced pressure. Crystallise the resulting oil by trituration in isopropyl ether. Recrystallise the resulting precipitate from a 9/1 cyclohexane/toluene mixture.

후처리

  1. customRemove the palladium-on-carbon
  2. filtrationby filtration
  3. customremove
  4. additionthe mixture of solvents
  5. customby evaporation under reduced pressure
  6. customCrystallise the resulting oil by trituration in isopropyl ether
  7. customRecrystallise the resulting precipitate from a 9/1 cyclohexane/toluene mixture

출처 및 근거

ORD 기록
ord-6ffcc5c8c2554855b473af381ae846df
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06919362B2

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