Triethyl phosphite → Diethyl(5-isoxazolylmethyl)phosphonate

HRID 1793855노트

반응식

HRID 1793855 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-18551b1b150942d5ae40a62ed09bc08a
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022706B2

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