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

HRID 1939688노트

반응식

HRID 1939688 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

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 azobis-isobutyronitrile 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.

후처리

  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

출처 및 근거

ORD 기록
ord-26be9e32081c4ba6a77a63b8dfa98cd8
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05696259

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