4-ethenyl-5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,6,7-tetramethyl-1-benzofuran-3(2H)-one → 4-ethyl-5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,6,7-tetramethyl-1-benzofuran-3(2H)-one

HRID 1850381노트

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HRID 1850381 반응식
[CH:1]([C:3]1[C:8]2[C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[O:11][C:7]=2[C:6]([CH3:15])=[C:5]([CH3:16])[C:4]=1[N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=2)[CH2:19][CH2:18]1)=[CH2:2]>[C].[Pd].C(O)C>[CH2:1]([C:3]1[C:8]2[C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[O:11][C:7]=2[C:6]([CH3:15])=[C:5]([CH3:16])[C:4]=1[N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:24]=[CH:25][C:26]([O:29][CH3:30])=[CH:27][CH:28]=2)[CH2:19][CH2:18]1)[CH3:2]

참가 물질

4

반응물 1

HCID 667602304-ethenyl-5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,6,7-tetramethyl-1-benzofuran-3(2H)-one

생성물 1

HCID 667596504-ethyl-5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,6,7-tetramethyl-1-benzofuran-3(2H)-one수율 36.5%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

5% palladium carbon (50% water content, 100 mg) was added to a solution of ethanol (5 mL) containing 4-ethenyl-5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,6,7-tetramethyl-1-benzofuran-3(2H)-one (100 mg, 0.246 mmol) synthesized in Reference Example 23, and the mixture was stirred under hydrogen atmosphere at room temperature for 20 hours. Palladium carbon was removed by filtration, and then the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 100:0 to 95:5) to give 36.7 mg of the title compound (yield: 36%).

후처리

  1. customsynthesized in Reference Example 23
  2. customPalladium carbon was removed by filtration
  3. customthe solvent was removed under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 100:0 to 95:5)

출처 및 근거

ORD 기록
ord-968c041f47864c9e9b033dbb12cca835
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957069B2

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