Bromine → Diethyl 4-Bromo-2-methylbenzylphosphonate

HRID 4915

반응식

HRID 4915 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 19797190Diethyl 4-Bromo-2-methylbenzylphosphonate

시약·촉매·용매 2

HCID 962Water용매HCID 10541Trimethyl Phosphate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d600937ba404454f851cb18c5c96b0b1
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242908

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