Phosphorus tribromide → 2-(2-Bromomethylphenylsulfanylmethyl)benzene

HRID 2416927

反応式

HRID 2416927 の反応式
[CH2:1]([S:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[CH2:15]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Br)(Br)[Br:18]>CCOCC>[Br:18][CH2:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[S:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24614Phosphorus tribromideHCID 10977293[2-(Benzylsulfanyl)phenyl]methanol

生成物 1

HCID 108808892-(2-Bromomethylphenylsulfanylmethyl)benzene収率 62.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of (2-Benzylsulfanyl) methanol 4 (120 mg, 0.522 mmol) in anhydrous Et2O was cooled to 4° C. A solution of PBr3 (49 μL, 0.52 mmol) in anhydrous Et2O was added dropwise, keeping the temperature below 10° C. The reaction was allowed to warm to ambient temperature and stirred for one hour. The reaction was filtered through silica gel (2.0 g) and washed with Et2O. The filtrate was washed with H2O saturated aqueous sodium bicarbonate and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give 95 mg of the named product as a yellow oil.

後処理

  1. customthe temperature below 10° C
  2. filtrationThe reaction was filtered through silica gel (2.0 g)
  3. washwashed with Et2O
  4. washThe filtrate was washed with H2O saturated aqueous sodium bicarbonate and brine
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-41ca3d8adcca4d3899a3b8500b8ba9a3
出典データセット
uspto-grants-2004_11
特許番号
US06825221B2

関連ノート

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