Triethyl phosphite → Phosphonic acid, P,P'-(1,4-phenylenebis(methylene))bis-, P,P,P',P'-tetraethyl ester

HRID 2222748

반응식

HRID 2222748 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9]Br)=[CH:5][CH:4]=1.[P:11]([O:18][CH2:19][CH3:20])([O:15][CH2:16][CH3:17])[O:12]CC>>[C:6]1([CH2:9][P:11](=[O:12])([O:15][CH2:16][CH3:17])[O:18][CH2:19][CH3:20])[CH:7]=[CH:8][C:3]([CH2:2][P:11](=[O:12])([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17])=[CH:4][CH:5]=1

참가 물질

3

반응물 2

HCID 31215Triethyl phosphiteHCID 693351,4-Bis(bromomethyl)benzene

생성물 1

HCID 78303Phosphonic acid, P,P'-(1,4-phenylenebis(methylene))bis-, P,P,P',P'-tetraethyl ester수율 89.1%

반응 조건

온도
130 °C

실험 절차

α, α′-Dibromo-p-xylene (5.28 g, 20 mmol, 1 equiv.) and triethyl phosphite (10.3 mL, 60 mmol, 3 equiv.) were placed in a flask with a magnetic stirring bar. A distillation apparatus was attached to collect ethyl bromide formed along with the reaction. The mixture was immersed in an oil bath and heated to 130° C. for 2 h. After cooling down, white crystal crushed out and recrystalized from hexane to give the product (6.74 g, 89% yield). 1H NMR (CDCl3) δ7.24 (s, 4H), 4.00 (m, 8H), 3.12 (d, 4H, J=20.2 Hz), 1.23 (t, 12H, J=7.0 Hz).

후처리

  1. customto collect ethyl bromide
  2. customformed along with the reaction
  3. customThe mixture was immersed in an oil bath
  4. temperatureAfter cooling down
  5. customwhite crystal crushed out and
  6. customrecrystalized from hexane

출처 및 근거

ORD 기록
ord-f43118ed414e415a8a83585a3fbbb3f5
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07371887B2

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