Triethyl phosphite → Diethyl 3-Nitrobenzylphosphonate

HRID 1295583ノート

反応式

HRID 1295583 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH2:7]Br)([O-:3])=[O:2].[P:12]([O:19]CC)([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15]>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH2:7][P:12](=[O:19])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 31215Triethyl phosphiteHCID 77568Benzene, 1-(bromomethyl)-3-nitro-

生成物 1

HCID 13675396Diethyl 3-Nitrobenzylphosphonate収率 68%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 3-nitrobenzyl bromide (17.3 g, 0.08 mol), triethyl phosphite (13.3 g, 0.08 mol) in toluene (200 mL) was stirred at reflux for 24 h. The reaction mixture was cooled and evaporated in vacuo. Chromatography of the residues on SiO2 eluting from 0–100% ethyl acetate in petroleum ether (60–80° C.) gave the title compound (14.8 g, 68%) as a yellow liquid.

後処理

  1. temperatureat reflux for 24 h
  2. temperatureThe reaction mixture was cooled
  3. customevaporated in vacuo

出典と根拠

ORDレコード
ord-0889e9f234de4bcb8da5c6f93585c8f8
出典データセット
uspto-grants-2007_07
特許番号
US07244726B2

反応ノート

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