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 2063790ノート

反応式

HRID 2063790 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-0885d77ee3f047e8bfea4829779af02f
出典データセット
uspto-grants-2012_10
特許番号
US08288390B2

反応ノート

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