反応 #5739

反応方程式

[1,1':3',1"-terphenyl]-2'-yl (chlorosulfonyl)carbamate

n-dodecyl alcohol

triethylamine

→

title compound

収率 42.5%

[1,1':3',1"-Terphenyl]-2'-yl[(dodecyloxy)sulfonyl]carbamate

収率 42.5%

溶媒

THF

THF

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   その他partitioned between H2O and EtOAc
3. 3
   乾燥The EtOAc layer was dried with MgSO4
4. 4
   その他evaporated
5. 5
   その他to give a white solid

実験手順

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.

出典