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Tetrahydrofuran → Diethyl 2-(3'-{[methyl-(1-phenylmethanoyl)-amino]methyl}biphenyl-4-ylmethyl)malonate

HRID 584913
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HRID 584913 반응식
[CH3:1][N:2]([CH2:11][C:12]1[CH:13]=[C:14]([C:18]2[CH:23]=[CH:22][C:21]([CH:24]=[C:25]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:20][CH:19]=2)[CH:15]=[CH:16][CH:17]=1)[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].C1COCC1>CO>[CH3:1][N:2]([CH2:11][C:12]1[CH:13]=[C:14]([C:18]2[CH:19]=[CH:20][C:21]([CH2:24][CH:25]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:22][CH:23]=2)[CH:15]=[CH:16][CH:17]=1)[C:3]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8028TetrahydrofuranHCID 22341469Diethyl 2-(3'-{[methyl-(1-phenylmethanoyl)amino]methyl}biphenyl-4-ylmethylene)malonate

생성물 1

HCID 22341493Diethyl 2-(3'-{[methyl-(1-phenylmethanoyl)-amino]methyl}biphenyl-4-ylmethyl)malonate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

700 mg (1.5 mmol) of diethyl 2-(3′-{[methyl-(1-phenylmethanoyl)amino]methyl}biphenyl-4-ylmethylene)malonate, 7 ml of THF and 1 ml of methanol are introduced into a three-necked flask under a stream of nitrogen. The reaction medium is degassed, 80 mg of palladium-on-charcoal (5%) are introduced and the mixture is hydrogenated under atmospheric pressure at room temperature for 20 hours. The reaction medium is filtered through Celite and evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a mixture of heptane and ethyl acetate (80/20). After evaporation of the solvents, 450 mg (63%) of the desired product are collected.

후처리

  1. customThe reaction medium is degassed
  2. addition80 mg of palladium-on-charcoal (5%) are introduced
  3. filtrationThe reaction medium is filtered through Celite
  4. customevaporated
  5. customThe residue obtained
  6. customis purified by chromatography on a column of silica
  7. washeluted with a mixture of heptane and ethyl acetate (80/20)
  8. customAfter evaporation of the solvents, 450 mg (63%) of the desired product
  9. customare collected

출처 및 근거

ORD 기록
ord-d3bc1959691e48688917894e1f76aa21
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06927228B2

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