반응 #53541

반응 방정식

4-aminophenol

di-tert-butyl-dicarbonate

diisopropylethylamine

→

4Boc-aminophenol

수율 96.1%

용매

THF

반응 조건

후처리

1. 1
   농축concentrated
2. 2
   세척the solution was washed with brine
3. 3
   건조dried (MgSO4)
4. 4
   농축concentrated
5. 5
   기타Purification on a silica gel column
6. 6
   세척eluting with 5% methanol/40% ethyl acetate hexane

실험 절차

To a solution of 4-aminophenol (10.9 g, 100 mmol) in THF (150 mL) cooled in an ice bath was added di-tert-butyl-dicarbonate (21.8 g, 100 mmol) followed by diisopropylethylamine (17.4 mL, 100 mmol). The mixture was stirred at room temperature overnight and concentrated. The residue was taken up in ethyl acetate and the solution was washed with brine, dried (MgSO4), and concentrated. Purification on a silica gel column eluting with 5% methanol/40% ethyl acetate hexane gave 4Boc-aminophenol (20.1 g, 96%). MS(NH3—CI): (M+NH3+H)=227.

출처