Triethyl phosphite → Diethyl (2,3,3-trifluro-2propenyl)phosphonate

HRID 949

反応式

HRID 949 の反応式
[F:1][C:2](=[C:5]([F:7])[F:6])[CH2:3]Br.[P:8]([O:15][CH2:16][CH3:17])([O:12][CH2:13][CH3:14])[O:9][CH2:10][CH3:11]>>[F:6][C:5]([P:8](=[O:15])([O:12][CH2:13][CH3:14])[O:9][CH2:10][CH3:11])([F:7])[C:2]([F:1])=[CH2:3].[F:1][C:2](=[C:5]([F:7])[F:6])[CH2:3][P:8](=[O:9])([O:12][CH2:13][CH3:14])[O:15][CH2:16][CH3:17]

参加物

4

反応物 2

HCID 31215Triethyl phosphiteHCID 106310791-Propene, 3-bromo-1,1,2-trifluoro-

生成物 2

HCID 53986716Diethyl (1,1,2-trifluoro-2-propenyl)phosphonate収率 11%HCID 54339468Diethyl (2,3,3-trifluro-2propenyl)phosphonate収率 14%

実験手順

A solution of 2,3,3-trifluoro-2-propenyl bromide (5.25 g, 30 mmol) and triethyl phosphite (4.15 g, 25 mmol) in acetonltrile (15 mL) was heated at reflux for overnight. The residue obtained after evaporation of the solvent was chromatographed over silica gel (hexanes/ethyl acetate/ethanol, 80/20/1) to give diethyl (1,1,2-trifluro-2-propenyl)phosphonate (0.8 g, 11%) and diethyl (2,3,3-trifluro-2-propenyl)phosphonate (1.0 g, 14%).

後処理

  1. temperatureat reflux for overnight
  2. customThe residue obtained
  3. customafter evaporation of the solvent
  4. customwas chromatographed over silica gel (hexanes/ethyl acetate/ethanol, 80/20/1)

出典と根拠

ORDレコード
ord-69bdc7c6a2fb4d4987a431b8e37f7f33
出典データセット
uspto-grants-1998_03
特許番号
US05723470

関連ノート

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