Water → Butyl(triphenyl)stannane

HRID 501915

반응식

HRID 501915 반응식
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]

참가 물질

5

반응물 3

HCID 962WaterHCID 8002Butyl bromideHCID 12540Triphenyltin Chloride

생성물 1

HCID 298153Butyl(triphenyl)stannane수율 85%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d616d122a69e4473b00fff81be3c6f46
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772417B2

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