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

HRID 1516873

반응식

HRID 1516873 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a36a48e2ff8f47c0a8bc18738a56eba3
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08227623B2

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