Bromine → Diethyl 4-Bromo-2-methylbenzylphosphonate

HRID 4915

反応式

HRID 4915 の反応式
[CH3:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8].[Br:17]Br>P(OC)(OC)(OC)=O.O>[CH3:1][C:2]1[CH:16]=[C:15]([Br:17])[CH:14]=[CH:13][C:3]=1[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8]

参加物

5

反応物 2

HCID 24408BromineHCID 112945Phosphonic acid, P-((2-methylphenyl)methyl)-, diethyl ester

生成物 1

HCID 19797190Diethyl 4-Bromo-2-methylbenzylphosphonate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 10541Trimethyl Phosphate溶媒

実験手順

10 g (42 mmol) of diethyl 2-methylbenzylphosphonate were dissolved in 60 ml of trimethyl phosphate and the solution was introduced into a flask protected from light and moisture. 16 g (0.05 mol) of Br2 were added dropwise, while stirring. The mixture was stirred at 90° C. for 15 hours and, after cooling, was diluted with 100 ml of water and extracted three times with 100 ml of n-hexane each time. The organic phase wa dried, concentrated and distilled.

後処理

  1. additionthe solution was introduced into a flask
  2. stirringThe mixture was stirred at 90° C. for 15 hours
  3. temperatureafter cooling
  4. extractionextracted three times with 100 ml of n-hexane each time
  5. customThe organic phase wa dried
  6. concentrationconcentrated
  7. distillationdistilled

出典と根拠

ORDレコード
ord-d600937ba404454f851cb18c5c96b0b1
出典データセット
uspto-grants-1993_09
特許番号
US05242908

関連ノート

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