Trimethyl phosphite → HCID 23208053、化合物

HRID 233440ノート

反応式

HRID 233440 の反応式
[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

参加物

3

反応物 2

HCID 8472Trimethyl phosphiteHCID 680214-Fluorobenzyl bromide

生成物 1

HCID 23208053HCID 23208053、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-55882e58f9774087b41d1694d6d8bf38
出典データセット
uspto-grants-1997_01
特許番号
US05593980

反応ノート

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