Triethyl phosphite → Diethyl 3-fluorobenzylphosphonate

반응식

[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5]Br.[P:10]([O:17]CC)([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]>>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]

참가 물질

반응물 2

HCID 31215Triethyl phosphite

HCID 680073-Fluorobenzyl bromide

생성물 1

HCID 11311157Diethyl 3-fluorobenzylphosphonate

반응 조건

온도: 160 °C

실험 절차

A mixture of 3-fluorobenzyl bromide (2 g) and triethyl phosphite (2.2 mL) was heated at 160° C. under nitrogen for 4 hours. After cooling, the were volatiles removed in vacuo and the residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100% to give diethyl (3-fluorobenzyl)phosphonate (2.46 g)

후처리

temperatureAfter cooling
customthe were volatiles removed in vacuo
customthe residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100%

출처 및 근거

ORD 기록: ord-28b00569f5bf49409286c1aa20be08a0
출처 데이터셋: uspto-grants-2016_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09290472B2

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