Triethyl phosphite → Diethyl [(2-iodophenyl)methyl]phosphonate

HRID 1516873

反応式

HRID 1516873 の反応式
[P:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:2]CC.[I:11][C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH2:14]Cl>C1(C)C(C)=CC=CC=1>[CH2:9]([O:8][P:1]([CH2:14][C:13]1[CH:16]=[CH:17][CH:18]=[CH:19][C:12]=1[I:11])(=[O:2])[O:5][CH2:6][CH3:7])[CH3:10]

参加物

4

反応物 2

HCID 31215Triethyl phosphiteHCID 1010641-(Chloromethyl)-2-iodobenzene

生成物 1

HCID 15166404Diethyl [(2-iodophenyl)methyl]phosphonate

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

Triethyl phosphite (ca 66.6 ml; 94% pure; ca. 396.8 mmol) and 2-iodobenzyl chloride 1 (100 g, 400 mmol; melted prior to use) were mixed with xylene (65 ml) in a 250 ml roundbottomed flask. The clear solution was heated to reflux while stirring for 24 hours. The reaction was followed by GC and 1H-NMR (CDCl3). The disappearing proton resonance of 2H, s, CH2I at 4.73 ppm and the new 2H, d, CH2PO(OEt)2 at 3.47 ppm were indicative for the progress of the reaction.

後処理

  1. temperatureThe clear solution was heated
  2. temperatureto reflux
  3. customCH2PO(OEt)2 at 3.47 ppm were indicative for the progress of the reaction

出典と根拠

ORDレコード
ord-a36a48e2ff8f47c0a8bc18738a56eba3
出典データセット
uspto-grants-2012_07
特許番号
US08227623B2

関連ノート

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