Water → Stannane, trimethyl(4-methylphenyl)-

HRID 36096

反応式

HRID 36096 の反応式
[C:1]1([CH3:9])[CH:6]=[CH:5][C:4]([Mg]Br)=[CH:3][CH:2]=1.[CH3:10][Sn:11](Cl)([CH3:13])[CH3:12].[Cl-].[NH4+].O>O1CCCC1>[C:1]1([CH3:9])[CH:6]=[CH:5][C:4]([Sn:11]([CH3:13])([CH3:12])[CH3:10])=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 962WaterHCID 14016Trimethyltin chlorideHCID 25517Ammonium ChlorideHCID 178418370HCID 178418370、化合物

生成物 1

HCID 617834Stannane, trimethyl(4-methylphenyl)-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

p-Tolylmagnesium bromide solution (Aldrich) (1.0M solution in diethyl ether) (53 ml, 0.0530 mol) was added dropwise to trimethyltin chloride (6.92 g, 0.0347 mol) in tetrahydrofuran (50 ml) under nitrogen at -10° C. The suspension was allowed to warm slowly to room temperature over 3 h then saturated ammonium chloride solution (10 ml) was added followed by sufficient water to dissolve the precipitate. The solution was extracted three times with diethyl ether-hexane (1:1). The combined organic phase was washed with brine, dried (magnesium sulfate) and the solvents removed in vacuo. Vacuum distillation of the residue afforded a colorless liquid (39°-40 ° C., 0.1 mm Hg) which was further purified by flash chromatography (silica gel, hexane) to give p-tolyltrimethyltin as a colorless liquid.

後処理

  1. dissolutionto dissolve the precipitate
  2. extractionThe solution was extracted three times with diethyl ether-hexane (1:1)
  3. washThe combined organic phase was washed with brine
  4. dry with materialdried (magnesium sulfate)
  5. customthe solvents removed in vacuo
  6. distillationVacuum distillation of the residue
  7. customafforded a colorless liquid (39°-40 ° C., 0.1 mm Hg) which
  8. customwas further purified by flash chromatography (silica gel, hexane)

出典と根拠

ORDレコード
ord-83450f01458d44f9ba9916ff859c6a4a
出典データセット
uspto-grants-1995_05
特許番号
US05412097

関連ノート

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