反応 #1206

ord-e403979772a141b9b46f8ea7de5203df

反応方程式

NCCO
ethanolamine
CCCCCCCCCCCCCCOCC1OC1(C)C
1-tetradecyloxy-3-methyl-2-butene oxide
CCCCCCCCCCCCCCOCC(NCCO)C(C)(C)O
title compound
収率 58.0%
CCCCCCCCCCCCCCOCC(NCCO)C(C)(C)O
3-(2-hydroxyethylamino)-4-tetradecyloxy-2-methyl-2-butanol
収率 58.0%

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 100-ml two-necked flask equipped with a stirrer and a dropping funnel
  2. 2
    温度While heating
  3. 3
    温度After heating
  4. 4
    workup.STIRRINGstirring the mixture further for 16 hours
  5. 5
    その他the resultant reaction mixture
  6. 6
    濃縮was concentrated under reduced pressure
  7. 7
    その他the resultant residue was purified by column chromatography on silica gel

実験手順

A 100-ml two-necked flask equipped with a stirrer and a dropping funnel was charged with 15.3 g (16.7 mmol) of ethanolamine and 5.0 g of ethanol. While heating and stirring the mixture at 80° C. in a nitrogen atmosphere, an ethanol solution of 5.00 g (16.7 mmol) of 1-tetradecyloxy-3-methyl-2-butene oxide was added dropwise over 3 hours. After heating and stirring the mixture further for 16 hours, the resultant reaction mixture was concentrated under reduced pressure, and the resultant residue was purified by column chromatography on silica gel, thereby obtaining 3.47 g (yield: 58%) of the title compound (IIc-4).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723497uspto-grants-1998_03