Iodine → Butyl(iodo)diphenylstannane

HRID 505953

反応式

HRID 505953 の反応式
[CH2:1]([Sn:5](C1C=CC=CC=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].[I:24]I>CO>[CH2:1]([Sn:5]([I:24])([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 807IodineHCID 298153Butyl(triphenyl)stannane

生成物 1

HCID 68417447Butyl(iodo)diphenylstannane

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

In a three-necked flask protected from light, butyltriphenyltin (21.05 g; 51.8 mmol) was dissolved in 50 mL of dry methanol. A solution of iodine (12.06 g; 47.5 mmol) in methanol was then added slowly. After stirring at room temperature during 16 hours, methanol was eliminated under vacuum. The residue was dissolved in petroleum ether and washed with a saturated aqueous solution of sodium thiosulphate. Organic layers were washed with a saturated NaCI solution and dried over MgSO4. Solvent was evaporated and the crude product was distilled using a Kugelrohr apparatus at 60° C. A colourless oil was obtained (22.2 g, 48.6 mmol).

後処理

  1. washwashed with a saturated aqueous solution of sodium thiosulphate
  2. washOrganic layers were washed with a saturated NaCI solution
  3. dry with materialdried over MgSO4
  4. customSolvent was evaporated
  5. distillationthe crude product was distilled
  6. customat 60° C
  7. customA colourless oil was obtained (22.2 g, 48.6 mmol)

出典と根拠

ORDレコード
ord-726b2b942a134ca4960de7ff4aff58ed
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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