Triethyl phosphite → Diethyl(5-isoxazolylmethyl)phosphonate

HRID 1168213노트

반응식

HRID 1168213 반응식
Br[CH2:2][C:3]1[O:7][N:6]=[CH:5][CH:4]=1.[CH2:8]([O:10][P:11]([O:15]CC)[O:12][CH2:13][CH3:14])[CH3:9]>>[O:7]1[C:3]([CH2:2][P:11](=[O:15])([O:12][CH2:13][CH3:14])[O:10][CH2:8][CH3:9])=[CH:4][CH:5]=[N:6]1

참가 물질

3

반응물 2

HCID 31215Triethyl phosphiteHCID 100349035-(Bromomethyl)-1,2-oxazole

생성물 1

HCID 11378989Diethyl(5-isoxazolylmethyl)phosphonate수율 92.8%

실험 절차

5-(Bromomethyl)isoxazole (5.38 g, 33.2 mmol) was stirred at 0° C. as triethylphosphite (5.7 mL, 33.2 mmol) was slowly added. The mixture was stirred at room temperature for 48 h, heated under reflux for 24 h, then concentrated. Purification by distillation at reduced pressure (bp 109-115° C./0.04 mm Hg) provided pure product as a colorless oil (6.75 g, 92.7%).

후처리

  1. additionwas slowly added
  2. temperatureheated
  3. temperatureunder reflux for 24 h
  4. concentrationconcentrated
  5. customPurification
  6. distillationby distillation at reduced pressure (bp 109-115° C./0.04 mm Hg)

출처 및 근거

ORD 기록
ord-c0c5ae0eb53f4f7cbe852c80dafc7cdd
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06624167B1

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