Trimethyl phosphite → HCID 23208053, 화합물

HRID 233440노트

반응식

HRID 233440 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[CH:4][CH:3]=1.[CH3:10][O:11][P:12]([O:15]C)[O:13][CH3:14]>>[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][P:12](=[O:15])([O:13][CH3:14])[O:11][CH3:10])=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 8472Trimethyl phosphiteHCID 680214-Fluorobenzyl bromide

생성물 1

HCID 23208053HCID 23208053, 화합물

실험 절차

A mixture of 4-fluorobenzyl bromide (4.86 g, 0.026M) and trimethylphosphite (10 mL, 0.085M) is heated at the reflux temperature for 48 hours. The solution is cooled and excess trimethylphosphite is removed under reduced pressure. The crude product is chromatographed over silica gel (40-63 mμ, 400 g, 45 mL fractions, ethyl acetate), eluting with ethyl acetate. Fractions 41-80 are combined, concentrated, and placed under vacuum for 36 hours. The product (4.52 g) is a colorless oil.

후처리

  1. temperatureis heated at the reflux temperature for 48 hours
  2. temperatureThe solution is cooled
  3. customexcess trimethylphosphite is removed under reduced pressure
  4. customThe crude product is chromatographed over silica gel (40-63 mμ, 400 g, 45 mL fractions, ethyl acetate)
  5. washeluting with ethyl acetate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-55882e58f9774087b41d1694d6d8bf38
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05593980

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