Water → Butyl(triphenyl)stannane

HRID 505952

反応式

HRID 505952 の反応式
Br[CH2:2][CH2:3][CH2:4][CH3:5].[C:6]1([Sn:12](Cl)([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.O>C(OCC)C>[CH2:2]([Sn:12]([C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)[CH2:3][CH2:4][CH3:5]

参加物

5

反応物 3

HCID 962WaterHCID 8002Butyl bromideHCID 12540Triphenyltin Chloride

生成物 1

HCID 298153Butyl(triphenyl)stannane収率 85%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

In a three-necked flask, a solution of 1-bromobutane (34.25 g, 250 mmol) in diethyl oxide was added on magnesium (7.3 g, 300 mmol) covered with dry diethyl oxide. When the addition was completed, the mixture was refluxed during one hour. This solution was then added to triphenyltin chloride (42.6 g, 110 mmol) in 150 mL of diethyl oxide and refluxed for 3 hours. The mixture was hydrolysed with a minimum of water, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated. Crystallization of the crude product in methanol gave a white solid (32.3 g, 93 mmol).

後処理

  1. additionWhen the addition
  2. temperaturethe mixture was refluxed during one hour
  3. temperaturerefluxed for 3 hours
  4. washwashed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated
  7. customCrystallization of the crude product in methanol

出典と根拠

ORDレコード
ord-5bacb774637e49378ccd4a3ba5aa4847
出典データセット
uspto-grants-2010_08
特許番号
US07781610B2

関連ノート

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