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Hydrogen Bromide → Phosphonic acid, (3-bromo-2-hydroxypropyl)-, diethyl ester

HRID 1706176
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HRID 1706176 반응식
[BrH:1].[O:2]1[CH2:13][CH:3]1[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8]>>[Br:1][CH2:13][CH:3]([OH:2])[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 260Hydrogen BromideHCID 98446Diethyl 2,3-epoxypropylphosphonate

생성물 1

HCID 10934659Phosphonic acid, (3-bromo-2-hydroxypropyl)-, diethyl ester수율 86.1%

실험 절차

(1)-(a) 47% Aqueous hydrobromic acid (82.8 g) was added dropwise to diethyl 2,3-epoxypropylphosphonate (77.6 g) under ice-cooling and with stirring over a five minutes interval. After the stirring was continued for an hour under ice-cooling and for 3 hours at ambient temperature, the reaction mixture was extracted with ethyl acetate (500 ml). The ethyl acetate layer was separated, washed three times with saturated aqueous sodium bicarbonate solution (200 ml and 100 ml×2) and twice with saturated aqueous sodium chloride solution (100 ml×2), dried over magnesium sulfate and evaporated to dryness to give oily diethyl 3-bromo-2-hydroxypropylphosphonate (94.7 g)

후처리

  1. temperaturecooling
  2. wait
After the stirring was continued for an hour under ice-
  • extractionthe reaction mixture was extracted with ethyl acetate (500 ml)
  • customThe ethyl acetate layer was separated
  • washwashed three times with saturated aqueous sodium bicarbonate solution (200 ml and 100 ml×2)
  • dry with materialtwice with saturated aqueous sodium chloride solution (100 ml×2), dried over magnesium sulfate
  • customevaporated to dryness
  • 출처 및 근거

    ORD 기록
    ord-e50c9f12300d45b497fb3b4f23662bed
    출처 데이터셋
    uspto-grants-1980_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04206156

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