Phosphorus tribromide → 3-(1-(Benzyloxyimino)ethyl)benzylbromide

HRID 2296970ノート

反応式

HRID 2296970 の反応式
[CH2:1]([O:8][N:9]=[C:10]([C:12]1[CH:13]=[C:14]([CH:17]=[CH:18][CH:19]=1)[CH2:15]O)[CH3:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Br)(Br)[Br:21]>C(OCC)C>[CH2:1]([O:8][N:9]=[C:10]([C:12]1[CH:13]=[C:14]([CH:17]=[CH:18][CH:19]=1)[CH2:15][Br:21])[CH3:11])[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 867586303-(1-(Benzyloxyimino)ethyl)benzylalcohol

生成物 1

HCID 734333223-(1-(Benzyloxyimino)ethyl)benzylbromide収率 194.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 2.55 g (10 mmol) of 3-(1-(benzyloxyimino)ethyl)benzylalcohol in 20 ml of dry diethyl ether was added dropwise 1.35 g (4.5 mmol) of phosphorous tribromide with ice-cooling. The mixture was removed from an ice bath and stirred at room temperature for 6 hours. To the reaction mixture were added ice water and diethyl ether. The mixture was stirred for 30 minutes and separated. The organic layer was washed successively with an about 5% aqueous solution of sodium bicarbonate and water, then dried and concentrated to obtain 2.78 g (8.74 mmol) of 3-(1-(benzyloxyimino)ethyl)benzylbromide.

後処理

  1. temperaturecooling
  2. customThe mixture was removed from an ice bath
  3. additionTo the reaction mixture were added ice water and diethyl ether
  4. stirringThe mixture was stirred for 30 minutes
  5. customseparated
  6. washThe organic layer was washed successively with an about 5% aqueous solution of sodium bicarbonate and water
  7. customdried
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-9185698488d54e1086fed725b3e01fad
出典データセット
uspto-grants-2002_12
特許番号
US06489487B1

反応ノート

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