반응 #5739

ord-77906ee1bea24ed3b1e739a1dc11b691

반응 방정식

O=C(NS(=O)(=O)Cl)Oc1c(-c2ccccc2)cccc1-c1ccccc1
[1,1':3',1"-terphenyl]-2'-yl (chlorosulfonyl)carbamate
CCCCCCCCCCCCO
n-dodecyl alcohol
CCN(CC)CC
triethylamine
CCCCCCCCCCCCOS(=O)(=O)NC(=O)Oc1c(-c2ccccc2)cccc1-c1ccccc1
title compound
수율 42.5%
CCCCCCCCCCCCOS(=O)(=O)NC(=O)Oc1c(-c2ccccc2)cccc1-c1ccccc1
[1,1':3',1"-Terphenyl]-2'-yl[(dodecyloxy)sulfonyl]carbamate
수율 42.5%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated in vacuo
  2. 2
    기타partitioned between H2O and EtOAc
  3. 3
    건조The EtOAc layer was dried with MgSO4
  4. 4
    기타evaporated
  5. 5
    기타to give a white solid

실험 절차

A solution of [1,1':3',1"-terphenyl]-2'-yl (chlorosulfonyl)carbamate (5.0 g, 12.9 mmoles) in 75 mL THF was added dropwise to a solution of n-dodecyl alcohol (2.4 g, 12.9 mmoles) and triethylamine (1.3 g, 12.9 mmoles) in 100 mL THF at ~15° C. under an atmosphere of N2. The mixture was allowed to warm to room temperature for 16 hours, then concentrated in vacuo and partitioned between H2O and EtOAc. The EtOAc layer was dried with MgSO4 and evaporated to give a white solid. Chromatography (SiO2, 10% EtOAc/hexanes) gave 2.95 g of the title compound, mp 124°-126° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05245068uspto-grants-1993_09