반응 #96157

반응 방정식

bis(dimethylamino)methane

2-furanmethanol

→

5-dimethylaminomethyl-2-furanmethanol

수율 94.0%

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   기타acetic acid was removed at 60° C. under reduced pressure
2. 2
   workup.ADDITIONIce (200 g) was added to the residue which
3. 3
   추출The mixture was extracted with ethyl acetate
4. 4
   기타the extracts were evaporated
5. 5
   workup.DISTILLATIONdistilled

실험 절차

A solution of bis(dimethylamino)methane (112 g, 1.1 mol) in acetic acid (200 ml) was added dropwise with cooling (10° C.) to a stirred solution of 2-furanmethanol (98 g, 1.0 mol) in acetic acid (1000 ml). The mixture was stirred at room temperature for 18 hours and acetic acid was removed at 60° C. under reduced pressure. Ice (200 g) was added to the residue which was made basic with 40% aqueous sodium hydroxide (with external cooling). The mixture was extracted with ethyl acetate and the extracts were evaporated and distilled to give 5-dimethylaminomethyl-2-furanmethanol (145 g, 94%) b.p. 92°-96° C./0.2 0.5 mmHg.

출처