z-1-[4-(2-Benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene → Ospemifene

HRID 1636936ノート

反応式

HRID 1636936 の反応式
C([O:8][CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][C:15](/[C:18](/[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[C:19](\[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)/[CH2:20][CH2:21][Cl:22])=[CH:14][CH:13]=1)C1C=CC=CC=1>C(OCC)(=O)C.C(O)C.[Pd]>[Cl:22][CH2:21][CH2:20]/[C:19](/[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)=[C:18](/[C:15]1[CH:14]=[CH:13][C:12]([O:11][CH2:10][CH2:9][OH:8])=[CH:17][CH:16]=1)\[C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

参加物

5

反応物 1

HCID 70116950z-1-[4-(2-Benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene

生成物 1

HCID 3036505Ospemifene

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Z-1-[4-(2-benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene (36 g, 0.08 mol) was dissolved in the mixture of ethyl acetate (350 ml) and ethanol (350 ml). Palladium on carbon (5%, 0.28 g) was added and the solution was flushed with hydrogen gas until there was not any starting compound left (thin layer chromatography). Palladium on carbon was filtered off through siliceous earth and the filtrate was evaporated. The residue was crystallized from the mixture of ethanol (155 ml) and water (65 ml). Yield 20 g.

後処理

  1. customthe solution was flushed with hydrogen gas until there
  2. waitleft (thin layer chromatography)
  3. filtrationPalladium on carbon was filtered off through siliceous earth
  4. customthe filtrate was evaporated
  5. customThe residue was crystallized from the mixture of ethanol (155 ml) and water (65 ml)

出典と根拠

ORDレコード
ord-af642dcf906445ceaa6d36d9fc8d886a
出典データセット
uspto-grants-2000_03
特許番号
US06037379

反応ノート

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