反応 #362092

反応方程式

Triethylamine

4-phenoxyphenol

butyl isocyanate

→

tan solid

収率 99.1%

Butylcarbamic acid 4-phenoxyphenyl ester

収率 99.1%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   抽出The solution was extracted with 1 N HCl
3. 3
   乾燥dried (MgSO4)
4. 4
   その他the solvent removed under reduced pressure

実験手順

Triethylamine (15 ml, 0.11 mol) was added dropwise under a nitrogen atmosphere to a solution of 4-phenoxyphenol (25.1 g, 0.14 mol) and butyl isocyanate (18 ml, 0.16 mol) in 400 ml of methylene chloride. After the addition, the solution was stirred overnight at room temperature. The solution was extracted with 1 N HCl, dried (MgSO4) and the solvent removed under reduced pressure to give 39.59 g of a tan solid. Recrystallization from diisopropyl ether gave the title compound as a white crystalline solid (21.01 g, 55%), mp 75°-77° C.

出典