Tributylstannane → 1-Fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene

HRID 54267

反応式

HRID 54267 の反応式
[F:1][C:2](S(C1C=CC=CC=1)(=O)=O)=[CH:3][C:4]([CH3:13])([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1)[CH3:5].[CH2:23]([SnH:27]([CH2:32][CH2:33][CH2:34][CH3:35])[CH2:28][CH2:29][CH2:30][CH3:31])[CH2:24][CH2:25][CH3:26].N(C(C)(C)C#N)=NC(C)(C)C#N>C1CCCCC1>[F:1][C:2]([Sn:27]([CH2:28][CH2:29][CH2:30][CH3:31])([CH2:32][CH2:33][CH2:34][CH3:35])[CH2:23][CH2:24][CH2:25][CH3:26])=[CH:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]([Cl:12])=[CH:10][CH:11]=1)([CH3:5])[CH3:13]

参加物

5

反応物 3

HCID 5948TributylstannaneHCID 6547AzobisisobutyronitrileHCID 538605131-Fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene

生成物 1

HCID 676323451-Fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

Under a nitrogen atmosphere, a stirring solution of 22.7 grams (0.067 mole) of 1-fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene, 42.0 grams (0.14 mole) of tributyltin hydride, and 0.5 gram (catalyst) of azobisisobutyronitrile in 700 mL of cyclohexane is heated at reflux for about three hours. After this time the reaction mixture is cooled to ambient temperature, and 125 mL of silica gel is added. The mixture is concentrated under reduced pressure, and the residue is subjected to column chromatography. The product-containing fractions are combined and concentrated under reduced pressure, yielding 1-fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene.

後処理

  1. temperatureat reflux for about three hours
  2. addition125 mL of silica gel is added
  3. concentrationThe mixture is concentrated under reduced pressure
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-beee978054c2486f921e37cce4ee1d7b
出典データセット
uspto-grants-1997_04
特許番号
US05622954

関連ノート

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